• 제목/요약/키워드: Isothermal DSC(differential scanning calorimetry)

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Amine Terminated Polyetherimide/에폭시 수지 시스템의 경화공정연구와 파괴인성에 관한 연구 (A Study on the Curing Behavior and Toughness of Amine Terminated Polyetherimide/Epoxy Resin System)

  • 김민영;이광기;김원호;황병선;김대식;박종만
    • 한국복합재료학회:학술대회논문집
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    • 한국복합재료학회 2002년도 춘계학술발표대회 논문집
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    • pp.147-150
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    • 2002
  • The cure kinetics of blends of epoxy (DGEBA:diglycidyl ether of bisphenol A)/anhydride (NMA:nadic methyl anhydride) resin with synthesized amino terminated polyetherimide (AT-PEI) were studied using differential scanning calorimetry (DSC) and Dynamic Mechanical Analysizer(DMA) under isothermal condition to determine the reaction parameters and gel-vitrification behavior. The fracture toughness of AT-PEI 20phr/epoxy resin system was improved over 224% and 42.5% more than neat epoxy resin and commercial PEI/Epoxy Resin System.

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CRYSTALLIZATION KINETICS OF Fe-Si-B-Cu-Nb AMORPHOUS RIBBONS

  • Zhou, S.X.;Ulvensoen, J.H.;Hoier, R.
    • 한국자기학회지
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    • 제5권5호
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    • pp.511-514
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    • 1995
  • The crystallization kinetics of $Fe_{73.5}Si_{13.5}B_{9}Cu_{1}Nb_{3}$ amorphous alloy has been investigated using differential scanning calorimetry (DSC). The crystallization process had two stages, i.e. precipitation of the $\alpha$-Fe(Si) solid solution and the tetragonal borides. The isothermal transformation data of the amorphous alloy has been fitted successfully to the generalized Johnson-Mehl-Avrami equation. The mean time exponent, n, obtained is close to 2.5. The value of n=2.5 may be interpreted as being due to a diffusion-controlled transformation process with a constant nucleation rate, one likely transformation mode for the crystallization of metallic amorphous alloys. The activation energy of the overall crystallization process deduced from the time to 50% crystallization are about 81 kcal/mole. The value is of the same order as those estimated from viscous flow.

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Cure Reactions of Epoxy/Anhydride/(Polyamide Copolymer) Blends

  • Youngson Choe;Kim, Wonho
    • Macromolecular Research
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    • 제10권5호
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    • pp.259-265
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    • 2002
  • The cure kinetics of blends of epoxy (DGEBA, diglycidyl ether of bisphenol A)/anhydride resin with polyamide copolymer, poly(dimmer acid-co-alkyl polyamine), were studied using differential scanning calorimetry (DSC) under isothermal condition. On increasing the amount of polyamide copolymer in the blends, the reaction rate was increased and the final cure conversion was decreased. Lower values of final cure conversions in the epoxy/(polyamide copolymer) blends indicate that polyamide hinders the cure reaction between the epoxy and the curing agent. The value of the reaction order, m, for the initial autocatalytic reaction was not affected by blending polyamide copolymer with epoxy resin, and the value was approximately 1.3, whereas the reaction order, n, for the general n-th order of reaction was increased by increasing the amount of polyamide copolymer in the blends, and the value increased from 1.6 to 4.0. A diffusion-controlled reaction was observed as the cure conversion increased and the rate equation was successfully analyzed by incorporating the diffusion control term for the epoxy/anhydride/(polyamide copolymer) blends. Complete miscibility was observed in the uncured blends of epoxy/(polyamide copolymer) up to 120 $^{\circ}C$, but phase separations occurred in the early stages of the curing process at higher temperatures than 120 "C. During the curing process, the cure reaction involving the functional group in polyamide copolymer was detected on a DSC thermogram.gram.

NPG 함량에 따른 DGEBA/MDA 계의 경화반응 속도론 (Cure Kinetics of DGEBA/MDA System with Various Contents of NPG)

  • 이홍기;김양림;이재영;김상욱
    • 한국재료학회지
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    • 제9권5호
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    • pp.467-472
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    • 1999
  • Neopentyl glycoI(NPG) 의 함량변화에 따른 diglycidyl ether of bisphenol A (DGEBA)/4,4' -methylene dianiline (MDA) 계의 등온적 경화거동을 DSC를 이용하여 분석하였다. DGEBA/MDA 계의 경화속도를 증가시키기 위하여 NPG를 첨가하였다. NPG 함량에 관계없이 전화율 곡선이 s-자 모양이었으며, 이것은 DGEBA/MDA/NPG 계의 경화반응이 자촉매 반응 메커니즘에 따른다는 것을 의미한다. NPG의 함량이 증가함에 따라 경화속도가 증가하였으며, 이것은 NPG가 가지고 있는 두 개의 hydroxyl 기가 촉매로 작용하기 때문이다.

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Cu-Zr-Al-Be 비정질합금의 결정화거동 및 속도론 (Crystallization Behavior and Kinetics of Cu-Zr-Al-Be Bulk Metallic Glass)

  • 김유찬;에릭플러리;석현광;차필령;이진규;이재철
    • 대한금속재료학회지
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    • 제46권6호
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    • pp.338-344
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    • 2008
  • The crystallization kinetics of the $Cu_{43}Zr_{43}Al_7Be_7$ bulk metallic glass were studied by differential scanning calorimetry(DSC) in the continuous heating and isothermal annealing modes. Only one major peak could be detected on the DSC traces of $Cu_{43}Zr_{43}Al_7Be_7$ bulk amorphous alloy, and the activation energy for crystallization corresponding to the peak determined by the Kissinger method was resulted of 239 kJ/mol. The isothermal kinetic, analyzed by the Johnson-Mehl-Avrami equation yielded values for the Avrami exponents in the range 1.69 to 2.37, which implied a crystallization governed by a three-dimensioned growth. Primary phases were essentially the cubic structure CuZr together with the $Cu_{10}Zr_7$ phase. At higher temperature, the CuZr disappeared while the $Cu_{10}Zr_7$ became predominant. After long term annealing at 731 K, the phases were $Cu_{10}Zr_7$, $Cu_2ZrAl$ and $Al_3Zr_5$.

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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    • 제17권1호
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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.

In Situ Detection of the Onset of Phase Separation and Gelation in Epoxy/Anhydride/Thermoplastic Blends

  • Choe, Young-Son;Kim, Min-Young;Kim, Won-Ho
    • Macromolecular Research
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    • 제11권4호
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    • pp.267-272
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    • 2003
  • The isothermal cure reactions of blends of epoxy (DGEBA, diglycidyl ether of bisphenol A)/anhydride resin with polyamide copolymer (poly(dimmer acid-co-alkyl polyamine)) or PEI were studied using differential scanning calorimetry (DSC). Rheological measurements have been made to investigate the viscosity and mechanical relaxation behavior of the blends. The reaction rate and the final cure conversion were decreased with increasing the amount of thermoplastics in the blends. Lower values of final cure conversions in the epoxy/thermoplastic blends indicate that thermoplastics hinder the cure reaction between the epoxy and the curing agent. Complete miscibility was observed in the uncured blends of epoxy/thermoplastics up to $120^{\circ}C$ but phase separations occurred in the early stages of the curing process at higher temperatures than $120^{\circ}C$. According to the rheological measurement results, a rise of G' and G" at the onset of phase separation is seen. A rise of G' and G" is not observed for neat epoxy system since no phase separation is seen during cure reaction. At the onset of phase separation the rheological behavior was influenced by the amount of thermoplastics in the epoxy/thermoplastic blends, and the onset of phase separation can be detected by rheological measurements.

Poly(N-vinylpyrrolidone)이 그래프트된 Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) 공중합체의 합성 및 결정화 거동 (Preparation and Crystallization Behavior of Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) Grafted with Poly(N-vinylpyrrolidone))

  • Wang, Wei;Zhang, Yu;Chen, Yanmo
    • 폴리머
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    • 제31권5호
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    • pp.385-392
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    • 2007
  • Poly (N-vinylpyrrolidone) (PVP) groups were grafted onto a poly(3-hydroxybutyrate-co-3-hydroryvalerate) (PHBV) backbone in order to modify its properties and synthesize a novel biocompatible copolymer. The crystallization behavior of PHBV and grafted PHBV was investigated by differential scanning calorimetry (DSC) and polarized optical microscopy (POM). During the cooling-induced crystallization process, the crystallization temperature and the crystallization rate of the grafted PHBV decreased with increasing PVP weight fraction. On the heating scans of all grafted PHBV samples, a new crystallization exothermic peak appeared at almost the same temperature, suggesting the operation of a recrystallization process, while the melting temperature ($T_m$) and the apparent enthalpy of fusion (${\Delta}H_f$) were not affected by graft modification. During the isothermal crystallization process at the same temperature, the presence of side PVP groups decreased the spherulitic growth rate and the spherulitic band spacing with increasing PVP weight fraction in samples.

Effect of A-Zeolite on the Crystallization Behavior of In-situ Polymerized Poly(ethylene terephthalate) (PET) Nanocomposites

  • Shin, Young-Hak;Lee, Wan-Duk;Im, Seung-Soon
    • Macromolecular Research
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    • 제15권7호
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    • pp.662-670
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    • 2007
  • The crystallization behavior and fine structure of poly(ethylene terephthalate) (PET)/A-zeolite nanocomposites were assessed via differential scanning calorimetry (DSC) and time-resolved small-angle X-ray scattering (TR-SAXS). The Avrami exponent increased from 3.5 to approximately 4.5 with increasing A-zeolite contents, thereby indicating a change in crystal growth formation. The rate constant, k, evidenced an increasing trend with increases in A-zeolite contents. The SAXS data revealed morphological changes occurring during isothermal crystallization. As the zeolite content increased, the long period and amorphous region size also increased. It has been suggested that, since PET molecules passed through the zeolite pores, some of them are rejected into the amorphous region, thereby resulting in increased amorphous region size and increased long period, respectively. In addition, as PET chains piercing into A-zeolite pores cannot precipitate perfect crystal folding, imperfect crystals begin to melt at an earlier temperature, as was revealed by the SAXS profiles obtained during heating. However, the spherulite size was reduced with increasing nanofiller content, because impingement between adjacent spherulites in the nanocomposite occurs earlier than that of homo PET, due to the increase in nucleating sites.

기계적 합금화 공정에 의한 Hf계 비정질 분말의 미세변형거동 관찰 (Micro-deformation behavior of Brittle Hf-based Metallic Glass during Mechanical Milling)

  • 김송이;이아영;차은지;권도훈;홍성욱;이민우;김휘준;이민하
    • 한국분말재료학회지
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    • 제25권3호
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    • pp.246-250
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    • 2018
  • In this study, we investigate the deformation behavior of $Hf_{44.5}Cu_{27}Ni_{13.5}Nb_5Al_{10}$ metallic glass powder under repeated compressive strain during mechanical milling. High-density (11.0 g/cc) Hf-based metallic glass powders are prepared using a gas atomization process. The relationship between the mechanical alloying time and microstructural change under phase transformation is evaluated for crystallization of the amorphous phase. Planetary mechanical milling is performed for 0, 40, or 90 h at 100 rpm. The amorphous structure of the Hf-based metallic glass powders during mechanical milling is analyzed using differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Microstructural analysis of the Hf-based metallic glass powder deformed using mechanical milling reveals a layered structure with vein patterns at the fracture surface, which is observed in the fracture of bulk metallic glasses. We also study the crystallization behavior and the phase and microstructure transformations under isothermal heat treatment of the Hf-based metallic glass.