• Title/Summary/Keyword: Differential scanning calorimeter

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Cure Behavior and Tensile Properties of Ethylidene Norbornene/endo-Dicyclopentadiene Blends (Ethylidene Norbornene/endo-Dicyclopentadiene 블렌드의 경화 거동 및 인장 특성)

  • Jung, Jong Ki;Choi, Jung Hwa;Yang, Guang;Park, Jongmoon;Kim, Donghak;Kim, Seonggil;Lee, Jong Keun;Oh, Myung-Hoon;Kim, Bongsuk;Bang, Daesuk
    • Polymer(Korea)
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    • v.39 no.3
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    • pp.506-513
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    • 2015
  • Ethylidene norbornene (ENB) and its blends with endo-dicyclopentadiene (endo-DCPD) were prepared and reacted via the ring-opening metathesis polymerization (ROMP) reaction with the $1^{st}$ and $2^{nd}$ generation Grubbs' catalysts. Dynamic exothermic behaviors during ROMP and tensile properties after ROMP were evaluated using a differential scanning calorimeter (DSC) and a universal testing machine (UTM) for the samples, respectively. It revealed that the ROMP rate was accelerated with the less contents of endo-DCPD and under the $2^{nd}$ generation catalyst. Also, the addition of endo-DCPD and the $1^{st}$ generation catalyst resulted in higher tensile modulus and strength but lower toughness. Gel fraction measurement and fracture surface observation were made to understand the tensile properties.

Thermal Stability and Cure Behavior of Waterborne Phenol-Formaldehyde Resin (수용성 페놀-포름알데히드 수지의 열안정성 및 경화거동)

  • Yoon, Sung Bong;Kim, Jin Woo;Cho, Donghwan
    • Journal of Adhesion and Interface
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    • v.7 no.1
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    • pp.16-22
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    • 2006
  • In this work, the effect of cure temperature and time on the thermal stability and the exothermic cure reaction peak of a waterborne resol-type phenol-formaldehyde resin, which may be used for preparing phenolic sheet molding compounds (SMC), has been investigated using a thermogravimetric analyzer and a differential scanning calorimeter. The weight loss of waterborne phenol-formaldehyde resin was mainly occurred at three temperature stages: near $200^{\circ}C,\;400^{\circ}C$, and $500^{\circ}C$. The carbon yield at $750^{\circ}C$ for the cured resin was about 62%~65%. Their thermal stability increased with increasing cure temperature and time. Upon cure, the exothermic reaction was taken placed in the range of $120^{\circ}C{\sim}190^{\circ}C$ and the maximum peak was found in between $165^{\circ}C$ and $170^{\circ}C$. The shape and the maximum of the exothermic curves depended on the given cure temperature and time. To remove $H_2O$ and volatile components, the uncured resin needed a heat-treatment at $100^{\circ}C$ for 60 min at least prior to cure or molding. Curing at $130^{\circ}C$ for 120 min made the exothermic peak of waterborne phenol-formaldehyde resin completely disappeared. And, post-curing at $180^{\circ}C$ for 60 min further improved the thermal stability of the cured resin.

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Studies on Cure Kinetics and Thermal Stability of Epoxy/Nylon 6 Blend (에폭시/나일론6 블랜드의 경화 동력학 및 열안정성에 관한 연구)

  • Kim, Dong-Kyu;Kim, Kwan-Woo;Han, Woong;Kwac, Lee-Ku;Kim, Byung-Joo
    • Applied Chemistry for Engineering
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    • v.26 no.5
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    • pp.538-542
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    • 2015
  • In this work, effects of the blend composition composed of 0, 10, 20, 30 and 40 wt% of nylon 6 to epoxy (diglycidylether of bisphenol-A, DGEBA) resin were investigated in terms of cure kinetics and thermal stability by differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). As the content of the nylon 6 increased, the maximum exothermic temperature ($T_{max}$) and the value of cure activation energy ($E_a$) decreased. The maximum exothermic temperature of the blending samples decreased with increasing in nylon 6 content, resulting in the decrease in curing activation energy of them due to the rapid curing reaction with epoxy resin in this system. From TGA analysis results of the DGEBA/nylon 6, the thermal stability based on the thermal stability index ($A^*{\cdot}K^*$) and integral procedure decomposition temperature (IPDT) increased with increase in the nylon 6 content. This was because of the combination of DGEBA and nylon 6 having good heat resistance, resulting in improving thermal stability of the DGEBA/nylon 6.

Effect of Ohmic Heating at Subgelatinization Temperatures on Thermal-property of Potato Starch (호화점 이하에서 옴가열이 감자 전분의 열적특성에 미치는 영향)

  • Cha, Yun-Hwan
    • The Korean Journal of Food And Nutrition
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    • v.25 no.4
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    • pp.1068-1074
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    • 2012
  • Ohmic heating uses electric resistance heat which occurs equally and rapidly inside of food when electrical current is flown into. In other study, we researched about soybean protein's characteristic changes by ohmic heating. Nevertheless treated same temperature, denaturation of soybean protein were accelerated by ohmic heating than conventional heating. In this time, we studied thermal property change of potato starch by ohmic heating besides conventional heating. For this purpose, potato starch was heated at same subgelatinization temperature by ohmic and conventional heating. And thermal properties were tested using DSC. Annealing of starch is heat treatment method that heated at 3~4% below the gelatinization point. DSC analysis results of this study, the $T_o$, $T_p$, $T_c$ of potato starch levels were increased, whereas $T_c{\sim}T_o$ was narrowed. This thermal property changes appear similar to annealing's result. It is thought the results shown in this study, because the heating from below the gelatinization point. 6, 12, 24, 72, and 120 hours heating at $55^{\circ}C$ for potato starch, $T_o$, $T_p$, $T_c$ values continue to increased with heating time increase. The gelatinization temperature of raw potato starch was $65.9^{\circ}C$ and the treated starch by conventional heating at $55^{\circ}C$ for 120 hr was $72^{\circ}C$, ohmic was $76^{\circ}C$. The gelatinization range of conventional (72 hr) was $10^{\circ}C$, ohmic was $8^{\circ}C$. In case of 24 hours heating at 45, 50, 55, 60, $65^{\circ}C$ for potato starch, the result was similar to before. $T_o$, $T_p$, $T_c$ values continue to increased and gelatinization range narrowed with heating temperature increase. In case of conventional heating at $60^{\circ}C$, the results of gelatinization temperature and range were $70.1^{\circ}C$ and $9.1^{\circ}C$. And ohmic were $74.4^{\circ}C$ and $7.5^{\circ}C$. When viewed through the results of the above, the internal structure of starch heated by ohmic heating was found that the shift to a more stable form and to increase the homology of the starch internal structure.

Analysis of Thermal Conductivities of Carbon/Phenolic and Silica/Phenolic Ablative Composites by Laser Pulse Method (레이저 섬광법을 이용한 Carbon/Phenolic 및 Silica/Phenolic 내열복합재료의 열전도도 분석)

  • Kim, H.Y.;Kim, P.W.;Hong, S.H.;Kim, Y.C.;Yeh, B.H.;Jung, B
    • Composites Research
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    • v.12 no.3
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    • pp.75-83
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    • 1999
  • The thermal properties of carbon/phenolic and silica/phenolic ablative composites were investigated by measuring the heat capacity, thermal diffusivity and thermal conductivity. The heat capacities of carbon/ phenolic and silica/phenolic composites were calculated from differential scanning calorimeter curve. The thermal diffusivities of carbon/phenolic and silica/phenolic composites were measured by the laser flash method with varying laminated direction, i.e., with laminar direction and across laminar direction. The thermal diffusivities decreased with increasing temperature. The thermal conductivities of carbon/phenolic and silica/phenolic composites were calculated using the heat capacity, density and thermal diffusivity. The thermal conductivities increased with increasing temperature. The thermal conductivity of with laminar direction is two times higher than that of across-laminar direction in carbon/phenolic composite due to the directionality of thermal conductivity of carbon fiber. The thermal conductivities of two dimensional fiber reinforced composites were analyzed using the conductivities of constituents and volume fraction of each constituent. The thermal conductivities of carbon fiber and silica fiber were calculated from thermal conductivities of carbon/phenolic and silica/phenolic composites. The thermal conductivities of carbon/phenolic and silica/phenolic composites at RT were predicted from thermal conductivities of fiber and resin with varying the volume fraction of fiber.

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Physical and Mechanical Properties of The Lignin-based Carbon Nanofiber-reinforced Epoxy Composite (에폭시 강화 리그닌 기반 나노탄소섬유 복합재료의 특성)

  • Youe, Won-Jae;Lee, Soo-Min;Lee, Sung-Suk;Kim, Yong Sik
    • Journal of the Korean Wood Science and Technology
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    • v.44 no.3
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    • pp.406-414
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    • 2016
  • The lignin-based carbon nanofiber reinforced epoxy composite has been prepared by immersing carbon nanofiber mat in epoxy resin solution in order to evaluate the physical and mechanical properties. The thermal and mechanical properties of the carbon nanofiber reinforced epoxy composite were analyzed using thermogravimetric analysis (TGA), differential scanning calorimeter (DSC) and tensile tester. It was found that the thermal properties of the carbon nanofiber reinforced epoxy composite improved, with its glass-transition temperature ($T_g$) increased from $90.7^{\circ}C$ ($T_g$ of epoxy resin itself) to $106.9^{\circ}C$. The tensile strengths of carbon nanofiber mats made from both lignin-g-PAN copolymer and PAN were 7.2 MPa and 9.4 MPa, respectively. The resulting tensile strength of lignin-based carbon nanofiber reinforced epoxy composite became 43.0 MPa, the six times higher than that of lignin-based carbon nanofiber mats. The carbon nanofibers were pulled out after the tensile test of the carbon nanofiber reinforced epoxy composite due to high tensile strength (478.8 MPa) of an individual carbon nanofiber itself as well as low interfacial adhesion between fibers and matrices, confirmed by the SEM analysis.

The Study on the Properties of Polypropylene/Nylon6 with Various Compatibilizers (Polypropylene/Nylon6 블렌드에서 이종의 상용화제에 따른 물성연구)

  • Kim, H.C.;Lee, K.Y.;Kim, H.I.
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.497-501
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    • 1999
  • The changes of properties were studied for the polypropylene(PP)/Nylon6 blends containing different kinds of compatibilizer made by either reactive extrusion of solution reaction. The compatibilizers were PP grafted with maleic anhydride (MAH) made by reactive extrusion and solution reaction. The grafted MAH contents were 0.3 wt %, and 2.7 wt %, respectively. The composition of the PP/nylon6 blend was fixed at 75/25 by weight. Blending was carried out with twin-screw extruder (L/D=30, ${\psi}=30$) at 300 rpm. As the content of PP-g-MAH was increased, the crystallization peak of Nylon6 decreased gradually then finally disappeared. Disappearance of crystallization peak of Nylon6 was mostly affected by grafted MAH content rather than the preparation method and the amount of compatibilizer. The portion of Nylon6 that could not crystallize in its normal crystallization temperature crystallized together with PP at the crystallization temperature of PP. So called concurrent crystallization was observed. Meanwhile two more peaks were observed during heating cycle. One was exothermic peak at $193^{\circ}C$ near to crystallization temperature of Nylon6, the other was endothermic peak at $215^{\circ}C$ that was $5^{\circ}C$ lower than normal endothermic peak of Nylon6. To analyze the peaks, nylon6 was annealed in the differential scanning calorimeter. As a result, the peak at $193^{\circ}C$ was crystallization peak of imperfect crystalline of Nylon6 and the other peak at $215^{\circ}C$ was melting peak of imperfect crystalline of nylon6.

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Effects of Annealing Temperature on Thermal Properties of Glycidyl Azide Polyol-based Energetic Thermoplastic Polyurethane (글리시딜아자이드계 열가소성 폴리우레탄의 열적특성에 대한 열처리 조건의 영향)

  • Kim, Jeong Su;Kim, Du Ki;Kweon, Jeong Ohk;Lee, Jae Myung;Noh, Si Tae;Kim, Sun Young
    • Applied Chemistry for Engineering
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    • v.24 no.3
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    • pp.305-313
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    • 2013
  • In this study, we investigated effects of thermal annealing on the thermal properties and microphase separation behaviors of glycidyl azide-based thermoplastic polyurethane elastomers (ETPE). The GAP-based ETPEs were characterized by attenuated total reflectance-fourier transform infrared spectroscopy (ATR-FTIR), differential scanning calorimeter (DSC), dynamic mechanical analysis (DMA), and gel permeation chromatography (GPC). The effects of annealing temperature conditions ($80{\sim}130^{\circ}C$, 1 h or 24 h) on the properties of the ETPEs were investigated. The intensity of azide group absorption peak of ATR-FTIR spectra and the solubility of ETPE for methylene chloride and dimethylformamide solvent decreased after the annealing at $130^{\circ}C$ for 1 h and at $105^{\circ}C$ for 24 h. With increasing the annealing temperature from $80^{\circ}C$ to $110^{\circ}C$, the high temperature rubbery plateau region of storage modulus curves from DMA thermogram for GAP-based ETPEs was extended to the higher temperature.

Ni0.5Zn0.4Cu0.1Fe2O4 Complex Ferrite Nanoparticles Synthesized by Chemical Coprecipitation Predicted by Thermodynamic Modeling

  • Kang, Bo-Sun;Park, Joo-Seok;Ahn, Jong-Pil;Kim, Kwang-Hyun;Tae, Ki-Sik;Lee, Hyun-Ju;Kim, Do-Kyung
    • Journal of the Korean Ceramic Society
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    • v.50 no.3
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    • pp.231-237
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    • 2013
  • Thermodynamic modeling of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite system has been adopted as a rational approach to establish routes to better synthesis conditions for pure phase $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite. Quantitative analysis of the different reaction equilibria involved in the precipitation of $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ from aqueous solutions has been used to determine the optimum synthesis conditions. The spinel ferrites, such as magnetite and substitutes for magnetite, with the general formula $MFe_2O_4$, where M= $Fe^{2+}$, $Co^{2+}$, and $Ni^{2+}$ are prepared by coprecipitation of $Fe^{3+}$ and $M^{2+}$ ions with a stoichiometry of $M^{2+}/Fe^{3+}$= 0.5. The average particle size of the as synthesized $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$, measured by transmission electron microscopy (TEM), is 14.2 nm, with a standard deviation of 3.5 nm the size when calculated using X-ray diffraction (XRD) is 16 nm. When $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite is annealed at elevated temperature, larger grains are formed by the necking and mass transport between the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite nanoparticles. Thus, the grain sizes of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ gradually increase as heat treatment temperature increases. Based on the results of Thermogravimetric Analysis (TGA) and Differential Scanning Calorimeter (DSC) analysis, it is found that the hydroxyl groups on the surface of the as synthesized ferrite nanoparticles finally decompose to $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ crystal with heat treatment. The results of XRD and TEM confirmed the nanoscale dimensions and spinel structure of the samples.

Explosion Properties and Thermal Stability of Reactive Organic Dust (반응성 유기물 분진의 폭발특성과 열안정성)

  • Han, Ou-Sup;Han, In-Soo;Choi, Yi-Rac;Lee, Keun-Won
    • Journal of the Korean Institute of Gas
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    • v.15 no.4
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    • pp.7-14
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    • 2011
  • Using 20 L spherical explosion vessel and differential scanning calorimeter (DSC), an experimental investigation was carried on explosion characteristics and thermal decomposition of some reactive organic dust. As the result, the minimum explosion concentration of Benzoyl peroxide (BPO), Phthalic anhydride (PA) and 1-Hydroxybenzotriazol (HBT) exist between 10 and 15 g/$m^3$, which indicates that their explosion sensitivity are high. The maximum Kst values of HBT, PA and 97 % BPO are 251, 146 and 80 [$bar{\cdot}m/s$], respectively and the explosion severity of HBT is the explosion class of St-2. The flame velocity was also calculated from the combustion time of dust and flame arrival time to estimate the flame propagation characteristics in a closed vessel. The decomposition temperature and heat of decomposition reaction for 97 % BPO and HBT are $107^{\circ}C$ (1025 J/g), $214^{\circ}C$ (1666 J/g), respectively and it was found that these low decomposition temperature and high released heat affect the explosion characteristics.