• Title/Summary/Keyword: non-isothermal DSC

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Glass Transition Temperature and Isothermal Physical Aging of PMMA Thin Films Incorporated with POSS (POSS를 함유한 PMMA 박막의 유리전이온도 및 등온 물리적 시효)

  • Jin, Sil-O;Lee, Jong-Keun
    • Polymer(Korea)
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    • v.36 no.4
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    • pp.507-512
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    • 2012
  • Thin (~650 nm) and ultrathin (~50 nm) films of neat PMMA and PMMA containing 5 wt% of methacryl-polyhedral oligomeric silsesquioxane were prepared in this work. The effects of film thickness and POSS on glass transition temperature ($T_g$) and isothermal physical aging were investigated by means of differential scanning calorimetry (DSC). $T_g$ depression was observed as film thickness was decreased and Ma-POSS molecules were incorporated. Enthalpy relaxation (${\Delta}H_{Relax}$) due to the isothermal physical aging was reduced by ultra-thin film thickness and the addition of Ma-POSS. KWW (Kohlrausch-Williams-Watts) equation was used to fit ${\Delta}H_{Relax}$ vs. aging time data providing the fitting parameters; maximum enthalpy recovery (${\Delta}H_{\infty}$), relaxation time (${\tau}$) and non-exponentiality parameter (${\beta}$).

Study on the Non-isothermal Crystallization Kinetics of Branched Polypropylene (분지형 폴리프로필렌의 비등온결정화 거동 연구)

  • Yoon, Kyung-Hwa;Shin, Dong-Yup;Kim, Youn-Cheol
    • Polymer(Korea)
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    • v.36 no.2
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    • pp.245-250
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    • 2012
  • Branched polypropylenes (PP) with long chain branch were prepared by solid state reaction with three different branching agent of 0.3 wt% content. The chemical structures, non-isothermal crystallization behavior and complex viscosity of the branched PP were investigated by FTIR, DSC, optical microscope, and dynamic rheological measurement. The chemical structure of the branched PP was confirmed by the existence of =C-H stretching peak of the branching agent at 3100 $cm^{-1}$. There was no distinct change in melting temperature in case of PP-D-0-3 and PP-F-0-3, but PP-H-0-3 indicated a decrease in melting temperature. The decrease in melting temperature was interpreted by the fact that the degradation reaction of PP was more dominant than branched reaction, and confirmed by a decrease in complex viscosity. The non-isothermal crystallization behavior of the branched PP was analyzed using by Avrami equation. The Avrami exponent of PP was 3, and the values of the branched PP with DVB and FS were below 3. The activation energy of PP calculated by Kissinger method was 25 kJ/mol, and there were no big difference in activation energies of the branched PPs compared to PP.

Catalyst Effects on Cross-linking of a Multi-Functional Fluoropolymer/Blocked-HMDI Blends (다기능성 함불소고분자/Blocked-HMDI 블렌드계의 가교화 반응에서의 촉매 영향)

  • Ahn, Won-Sool
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.13 no.5
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    • pp.2408-2413
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    • 2012
  • Effects of stanous catalyst on the cross-linking reaction characteristics of multi-functional fluoropolymer with blocked-hexamethylene diisocyanate(HMDI) were studied by dynamic DSC and non-isothermal thermogravimetric analysis (TGA). Results showed that cross-linking reaction occurred around $230-250^{\circ}C$ aftr the solvent and phenol, blocking agent, were removed upto the $150^{\circ}C$. It was considered that the reaction mechanism of the multi-functional fluoropolymer with HMDI might not be changed by the catalyst, however, the reaction rate became extremely faster upto to 100 times, showing the change of activation energy 81.8 kJ/mol for non-catalytic system to 61.7 kJ/mol for 1 phr catalytic system.

A Synthesis of Spherical Shape $TiO_2-SiO_2$ Complex via Solvothermal Process and Thermal Properties at Non-Isothermal (용매열합성을 이용한 구형 $TiO_2-SiO_2$ 복합체 제조 및 열적특성)

  • Cho Tae-Hwan;Park Seong-Jin
    • Journal of the Microelectronics and Packaging Society
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    • v.12 no.2 s.35
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    • pp.141-147
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    • 2005
  • Nanomaterial $TiO_2-SiO_2$ was synthesized by hydrolysis and condensation process using 2-propanol(2-PrOH) and was characterized by FT-IR, DSC, XRD and FE-SEM. FT-IR spectra were measured to investigate Ti-0-Si absorption peak. DSC thermal analysis results appllied to Ozawa equation were used to calculate to activation energy of crystallization. It was found that the changes of X-ray diffraction patterns and FWHM obtained XRD measurement depended on calcination temperature. In FE-SEM analysis, particle size changed by quantity changes of Ti-alkokide.

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Crystallization Behaviour of PP and Carbon Nanofibre Blends

  • Chatterjee, A.;Deopura, B.L.
    • Fibers and Polymers
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    • v.4 no.3
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    • pp.102-106
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    • 2003
  • Crystallization behaviour of blends of different MFI isotactic polypropylenes (PP), and blends of PP with carbon nanofibre have been investigated by DSC and polarizing optical microscope. Both higher MFI PP component and the carbon nanofibre in the blend influence the nucleation activity of the melt during non-isothermal crystallization. In presence of carbon nanofibre, the sherulitic growth rate is highly disturbed. The calculation of nucleation activity indicates that carbon nanofibres act as active substrate for heterogeneous nucleation.

Evaluation of Thermal Property and Fluidity with Underfill for BGA Package (BGA 패키지를 위한 언더필의 열적 특성과 유동성에 관한 연구)

  • Noh, Bo-In;Lee, Bo-Young;Kim, Soo-Jung;Jung, Seung-Boo
    • Journal of Welding and Joining
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    • v.24 no.2
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    • pp.57-63
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    • 2006
  • In this study, the curing kinetics and thermal degradation of underfill were investigated using differential scanning calorimetry (DSC) and thermo gravimetry analysis (TGA). The mechanical and thermal properties of underfill were characterized using dynamic mechanical analysis (DMA) and thermo-mechanical analysis (TMA). Also, we presented on underfill dispensing process using Prostar tool. The non-isothermal DSC scans at various heating rates, the exothermic reaction peak became narrower with increasing the heating rate. The thermal degradation of underfill was composed of two processes, which involved chemical reactions between the degrading polymer and oxygen from the air atmosphere. The results of fluidity phenomena were simulated using Star CD program, the fluidity of the underfills with lower viscosity was faster.

Non-isothermal Crystallization Behavior of Poly(glycolide-co-ε-caprolactone-co-L-lactide) Block Copolymer (생체분해성 Poly(glycolide-co-ε-caprolactone-co-L-lactide) 블록 공중합물의 비등온 결정화 거동에 관한 연구)

  • Choi, Sei-Young;Song, Seung-Ho
    • Elastomers and Composites
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    • v.49 no.1
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    • pp.13-23
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    • 2014
  • In this work, glycolide, L-lactide and ${\varepsilon}$-caprolactone monomers were polymerized into the triblock copolymers by two step polymerization method and their non-isothermal crystallization behaviors were studied by combination of modified Avrami and Ozawa formula for further analysis of their behaviors. The result showed that PGCLA21 gave the highest value for supercooling analysis and super cooling degree increased with L-lactide content. Crystallization velocity constant, however, showed no significant change. The result of cooling function in specific relative crystallization degree showed that the increase of L-lactide content made an effect on the more enhancement of crystallization velocity of the PGCLA than PGCL. The result of big logF(T) value with the L-lactide content above critical point for PGCLA41 and PGCLA21 showed that bigger cooling velocity needed to gain same crystal size compared with PGCL. This means that it gives negative effect in the increase of crystallization velocity.

Effects of Catalysts on the Adhesive Properties for Flip Chip Bonding (플립칩 본딩용 접착제 특성에 미치는 촉매제의 영향)

  • Min, Kyung-Eun;Lee, Jun-Sik;Yoo, Se-Hoon;Kim, Mok-Soon;Kim, Jun-Ki
    • Korean Journal of Materials Research
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    • v.20 no.12
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    • pp.681-685
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    • 2010
  • The application of flip chip technology has been growing with the trend of miniaturization of electronic packages, especially in mobile electronics. Currently, several types of adhesive are used for flip chip bonding and these adhesives require some special properties; they must be solvent-free and fast curing and must ensure joint reliability against thermal fatigue and humidity. In this study, imidazole and its derivatives were added as curing catalysts to epoxy resin and their effects on the adhesive properties were investigated. Non-isothermal DSC analyses showed that the curing temperatures and the heat of reaction were dependent primarily on the type of catalyst. Isothermal dielectric analyses showed that the curing time was dependent on the amount of catalysts added as well as their type. The die shear strength increased with the increase of catalyst content while the Tg decreased. From this study, imidazole catalysts with low molecular weight are expected to be beneficial for snap curing and high adhesion strength for flip chip bonding applications.

A Study on Effects of Vulcanization Systems on Cross-linking and Degradation Reactions of NR/CR Blends Using Dynamic DSC and TGA (Dynamic DSC와 TGA를 이용한 NR/CR 고무블렌드의 가황시스템이 가교 및 열화반응에 미치는 영향 연구)

  • Min, Byung-kwon;Park, DongRyul;Ahn, WonSool
    • Korean Chemical Engineering Research
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    • v.47 no.2
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    • pp.169-173
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    • 2009
  • Effects of variations sulfur/accelerator ratio on cross-linking and thermal degradation behavior of NR/CR rubber compounds were studied using both dynamic DSC and non-isothermal TGA. DSC thermograms of the given samples were obtained with several different heating rates, and after cross-liked in DSC, TGA thermograms with the same samples also obtained. Kissinger analysis was applied to assess the activation energies for the cross-linking and thermal decomposition processes. Results showed that the formation and thermal decomposition reaction of the samples occurred in the overall temperature range of $120{\sim}180^{\circ}C$ and $350{\sim}450^{\circ}C$, respectively, exhibiting that data could be well-fittable by Kissinger method. Furthermore, formation activation energy by DSC was estimated as $83.0{\pm}5.0kJ/mol$, which was much smaller than that of degradation by TGA, $147.0{\pm}2.0kJ/mol$. From these results, it was considered that, although variations of sulfur/accelerator ratio in the present experiments affected little on the formation mechanism and/or thermal degradation, they could play roles as the catalysts which lower the activation energy of formation. Because of stabilization after formation reaction, however, they have no more effects on the lowering the activation energy, showing higher values when decomposition, caused by main-chain scissions.

Study on the Physical and Rheological Properties of Nylon66/MWCNT Composites (나일론66/MWCNT 복합체 물성 및 유변학적 특성 연구)

  • Kim, Do Eui;Kim, Youn Cheol
    • Applied Chemistry for Engineering
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    • v.24 no.2
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    • pp.214-218
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    • 2013
  • Nylon66/multi-walled carbon nano tube (MWCNT) composites were fabricated by twin screw extruder. The contents of MWCNT were 1, 3, 5, and 7 wt%. Thermal properties, dispersion, rheological and impact properties were measured by DSC, TGA, X-ray diffraction (XRD), SEM, Dynamic rheometer, and Izod impact tester. The effect of MWCNT on the non-isothermal crystallization of Nylon66 was confirmed by DSC. The complex viscosity at low frequency and the shear thinning tendency of the composites increased with MWCNT content. An increase in the elasticity was confirmed from the decrease in the slop of G'-G" plot. Izod impact strengths of the composites were analyzed as a measure of mechanical properties, which indicated that the composites exhibit a 60% enhancement for the impact strength when 3 wt% MWCNT was added. The dispersion of MWCNT within Nylon66/MWCNT composites was also checked by SEM.