• Title/Summary/Keyword: Thermal curing

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Effects of Equivalent Weight of Epoxy Resins and Content of Catalyst on the Curing Reaction in Cationic Catalyst/Epoxy Cure System (양이온 촉매/에폭시 경화계에서 에폭시 수지의 당량 및 촉매 함량이 경화반응에 미치는 영향)

  • Kim, Youn Cheol;Park, Soo-Jin;Lee, Jae-Rock
    • Applied Chemistry for Engineering
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    • v.8 no.6
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    • pp.960-966
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    • 1997
  • The effects of epoxy resins and content of catalyst on the cure characteristics were studied by FT-IR, DSC and dynamic viscometer for the thermal properties and rheological properties of the catalytic (N-Benzylpyrazinium hexafluoroantimonate, BPH) epoxy thermosetting system. Compared with DSC results of DEGBF containing 0.5wt% BPH, the DSC thermograms of DGEBA containing 0.5wt% BPH indicated that the reaction was faster than that of DGEBF/BPH and the conversion rate of DGEBA/BPH was high in the initial stage of the reaction. As the concentration of BPH increases, the reaction and conversion rates show similar value in both the cases. The influence of hydroxyl group of epoxy resin on gel point defined from the crossover point of storage modulus (G') and loss modulus (G") could be explained by the formation of 3-dimensional network in the initial stage owing to the curing reaction between epoxides and hydroxyl groups of epoxy resin. This was consistent with the gel point obtained from DSC, FT-IR and moduli crossover. The activation energy (Et) obtained from the crossover point (G'/G"=1) are $31-39kJ.mol^{-1}$ for various BPH compositions in case of two epoxy systems.

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Synthesis and Curing Behaviors of Polyisoimide Oligomers with Ethynyl End Groups (Ethynyl 말단기를 갖는 Polyisoimide 올리고머의 합성 및 이들의 경화거동에 관한 연구)

  • Choi, Seok Woo;Kim, Bo Ock;Kim, Ji-Heung;Nam, Sung Woo;Jeon, Boong Soo;Kim, Young Jun
    • Polymer(Korea)
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    • v.38 no.6
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    • pp.774-781
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    • 2014
  • Acetylenic or phenylethynyl end-capped polyisoimide oligomers ($M_w$ 2500 g/mol, 5000 g/mol) based upon 4,4'-diamino diphenyl ether (4,4'-ODA)/4,4'-oxydiphthalic anhydride (ODPA) and 4,4'-ODA/3,3',4,4'-benzophenone tetracarboxylic acid dianhydride (BTDA) were synthesized by using 4-ethynylaniline (4-EA) or 4-phenylethynyl phthalic anhydride (4-PEPA) as an end capper. The incorporation of ethynyl groups were confirmed by FTIR spectroscopy. The isomerization temperature was influenced by molecular weight as well as the backbone structure of polyisoimides oligomers. Thus, polyisoimide oligomers with molecular weight of 2500 g/mol was found to be imidized at temperature $10^{\circ}C$ lower than that for the oligomers with molecular weight of 5000 g/mol. The crosslinking reaction of ethynyl groups occurred at a higher temperature than that for the isoimide/imide isomerization reaction. These two reactions were totally or partially overlapped on the DSC thermograms for the polyisoimide oligomer end-capped with 4-EA. Kinetics of thermal imidization and crosslinking reactions for the 4,4'-ODA/ODPA polyisoimide oligomers end-capped with 4-PEPA were investigated by performing dynamic DSC experiments at heating rate of $10^{\circ}C/min$. The activation energy and pre-exponential factors were 141 kJ/mol and $1.45{\times}10^{13}min^{-1}$ for the imidization reaction and 177 kJ/mol and $2.90{\times}10^{13}min^{-1}$ for the crosslinking reaction, respectively.

Study on the Improved Abrasion Resistance of Polycarbonate Substrate by UV-curable Organic/Inorganic Hybrid Coatings (자외선 경화형 유기/무기 복합코팅에 의한 폴리카보네이트의 내마모성 향상 연구)

  • 윤석은;우희권;김동표
    • Polymer(Korea)
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    • v.24 no.3
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    • pp.389-398
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    • 2000
  • Transparent, abrasion resistant coatings with 4~13 ${\mu}{\textrm}{m}$ thickness were prepared by spin-coating on polycarbonates with organic/inorganic hybrid solutions, followed by UV curing and heat treatment at 12$0^{\circ}C$ for 12 hours. The coating solutions were composed of inorganic phase and organic phase in 0:100, 20:80, 30:70, 50:50, 80:20 wt% ratios, respectively, mixed with photoinitiator, senaitizer and surfactant. The inorganic phase was formed by sol-gel reaction of TEOS and silane coupling agent MPTMS in 1 : 2 or 2 : 1 molar ratios, the organic phase consisted of difunctional urethane acrylate oligomeric resin, multifunctional acrylate TMPTA and HDDA in 4 : 3 : 3 wt% ratio. The coating systems were investigated by FT-IR, $^{29}$ Si-NMR spectra. In addition, TGA/DSC for thermal analysis and SEM, AFM observation for coated surface were examined. Gererally, the homogeneity of phases, the surface smoothness of coating and abrasion resistance were improved with the higher content of inorganic component. Namely, coating system with below 10 $\AA$ surface roughness and T$_{g}$ of 15$0^{\circ}C$ showed only 10% decrease in light transmittance after abrasion test, whereas uncoated polycarbonate substrate exhibited 46% decrease..

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Heat Performance of Rapid Hardening Nano-Cementitious Composite for Repairing of Concrete Structures (콘크리트 구조물 보수를 위한 초속경 나노-시멘트 복합체의 발열성능)

  • Cho, Sanghyeon;Lee, Heeyoung;Yu, Wonjun;Kim, Donghwi;Chung, Wonseok
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.8 no.4
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    • pp.421-428
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    • 2020
  • Recently, excellent thermal and electrical performance of cementitious composites by mixing nano materials are being studied. The purpose of this study is to research the heat generation and power consumption of rapid hardening nano-cementitious composites. The experiment was carried out after setting the rapid hardening cementitious material, curing day, and supply voltage as parameters. Rapid hardening nano-cementitious materials were classified into cement paste, mortar, and concrete The heat performance of all rapid hardening nano-cementitious composites in curing 1 day has increased over 10℃. The rapid hardening nano-cementitious composites can exhibit heat performance within 1 day. The heat performance of the rapid hardening nano-cementitious composites is maintained after 28 days.

Room-temperature Bonding and Mechanical Characterization of Polymer Substrates using Microwave Heating of Carbon Nanotubes (CNT 마이크로파 가열을 이용한 고분자 기판의 상온 접합 및 기계적 특성평가)

  • Sohn, Minjeong;Kim, Min-Su;Ju, Byeong-Kwon;Lee, Tae-Ik
    • Journal of the Microelectronics and Packaging Society
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    • v.28 no.2
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    • pp.89-94
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    • 2021
  • The mechanical reliability of flexible devices has become a major concern on their commercialization, where the importance of reliable bonding is highlighted. In terms of component materials' properties, it is important to consider thermal damage of polymer substrates that occupy large area of the flexible device. Therefore, room temperature bonding process is highly advantageous for implementing flexible device assemblies with mechanical reliability. Conventional epoxy resins for the bonding still require curing at high temperatures. Even after the curing procedure, the bonding joint loses flexibility and exhibits poor fatigue durability. To solve this problems, low-temperature and adhesive-free bonding are required. In this work, we develop a room temperature bonding process for polymer substrates using carbon nanotube heated by microwave irradiations. After depositing multiple-wall carbon nanotubes (MWNTs) on PET polymer substrates, they are heated locally with by microwave while the entire bonding specimen maintains room temperature and the heating induces mechanical entanglement of CNT-PET. The room temperature bonding was conducted for a PET/CNT/PET specimen at 600 watt of microwave power for 10 seconds. Thickness of the CNT bonding joint was very thin that it obtains flexibility as well. In order to evaluate the mechanical reliability of the joint specimen, we performed lap shear test, three-point bending test, and dynamic bending test, and confirmed excellent joint strength, flexibility, and bending durability from each test.

Enhancement in the photocurrent of ZnO nanoparticles by thermal annealing

  • Byun, Kwang-Sub;Cho, Kyuong-Ah;Jun, Jin-Hyung;Seong, Ho-Jun;Kim, Sang-Sig
    • Journal of IKEEE
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    • v.13 no.1
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    • pp.57-64
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    • 2009
  • The optoelectrical characteristics of the ZnO nanoparticles (NPs) annealed in vacuum or oxygen condition from $200^{\circ}C$ to $600^{\circ}C$ were examined. Increased on-off ratio (or, the ratio of photocurrent to dark current) was observed when they were annealed at $300^{\circ}C$, $400^{\circ}C$ and $500^{\circ}C$ with the values enhanced about 4 orders compared to the as-prepared ZnO NPs in both annealing conditions, while the maximum efficiency was shown at the annealing temperature of $600^{\circ}C$ for the ZnO NPs annealed in vacuum with the value of 29.8 mA/W and at the temperature of $500^{\circ}C$ for those annealed in oxygen condition with the value of 40.3 mA/W. Photoresponse behavior of the ZnO NPs annealed in oxygen showed the sharp increase right after the ir exposure to the light followed by the slow decay and saturation during steady illumination, differing from the ZnO NPs annealed in vacuum which only exhibited the gradual increase. This difference occurred due to the curing effect of the oxygen vacancies. SEM images indicated no change in their morphologies with annealing, indicating the change in their internal structures by annealing, and most remarkably at $600^{\circ}C$. As for their photoluminescence(PL) spectra, the decrease of the deep-level(DL) emission was observed when they were annealed in oxygen at $400^{\circ}C$, and not at $200^{\circ}C$ and $600^{\circ}C$.

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용액공정을 이용한 SiOC/SiO2 박막제조

  • Kim, Yeong-Hui;Kim, Su-Ryong;Gwon, U-Taek;Lee, Jeong-Hyeon;Yu, Yong-Hyeon;Kim, Hyeong-Sun
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2009.11a
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    • pp.36.2-36.2
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    • 2009
  • Low dielectric materials have been great attention in the semiconductor industry to develop high performance interlayer dielectrics with low k for Cu interconnect technology. In our study, the dielectric properties of SiOC /SiO2 thin film derived from polyphenylcarbosilane were investigated as a potential interlayer dielectrics for Cu interconnect technology. Polyphenylcarbosilane was synthesized from thermal rearrangement of polymethylphenylsilane around $350^{\circ}C{\sim}430^{\circ}C$. Characterization of synthesized polyphenylcarbosilane was performed with 29Si, 13C, 1H NMR, FT-IR, TG, XRD, GPC and GC analysis. From FT-IR data, the band at 1035 cm-1 is very strong and assigned to CH2 bending vibration in Si-CH2-Si group, indicating the formation of the polyphenylcarbosilane. Number average of molecular weight (Mn) of the polyphenylcarbosilane synthesized at $400^{\circ}C$ for 6hwas 2, 500 and is easily soluble in organic solvent. SiOC/SiO2 thin film was fabricated on ton-type silicon wafer by spin coating using 30wt % polyphenylcarbosilane incyclohexane. Curing of the film was performed in the air up to $400^{\circ}C$ for 2h. The thickness of the film is ranged from $1{\mu}m$ to $1.7{\mu}m$. The dielectric constant was determined from the capacitance data obtained from metal/polyphenylcarbosilane/conductive Si MIM capacitors and show a dielectric constant as low as 2.5 without added porosity. The SiOC /SiO2 thin film derived from polyphenylcarbosilane shows promising application as an interlayer dielectrics for Cu interconnect technology.

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Fundamental Properties of Cement Composites Containing Lightly Burnt MgO Powders (저온 소성한 MgO 분말을 혼입한 시멘트 복합체의 기초 물성)

  • Jang, Bong-Seok;Kwon, Yong-Gil;Choi, Seul-Woo;Lee, Kwang-Myong
    • Journal of the Korea Concrete Institute
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    • v.23 no.2
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    • pp.225-233
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    • 2011
  • The volume change in concrete takes place with changes in temperature and water content immediately after concrete casting. In the early age stage, the thermal and drying shrinkages can cause cracks that are very crucial to the durability of concrete. It was reported that when the cement with lightly-burnt MgO powder was used, the shrinkage of concrete can be reduced. This study investigates fundamental properties of cement composites with lightly burnt MgO powder by performing various experiments. The stability test results verified that MgO powder in cement composites does not cause any abnormal expansion. Also, the hydrate product analysis results obtained from MgO cement paste showed that MgO powder reduces the shrinkage at the longterm ages. In addition, the cement composites containing the proper amount of MgO powder could improve compressive strength. Finally, the shrinkage reduction from using MgO powder can be optimized by increasing MgO replacement level and curing temperature.

Polarity-tuned Gel Polymer Electrolyte Coating of High-voltage LiCoO2 Cathode Materials

  • Park, Jang-Hoon;Cho, Ju-Hyun;Kim, Jong-Su;Shim, Eun-Gi;Lee, Yun-Sung;Lee, Sang-Young
    • Journal of the Korean Electrochemical Society
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    • v.14 no.2
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    • pp.117-124
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    • 2011
  • We demonstrate a new surface modification of high-voltage lithium cobalt oxide ($LiCoO_2$) cathode active materials for lithium-ion batteries. This approach is based on exploitation of a polarity-tuned gel polymer electrolyte (GPE) coating. Herein, two contrast polymers having different polarity are chosen: polyimide (PI) synthesized from thermally curing 4-component (pyromellitic dianhydride/biphenyl dianhydride/phenylenediamine/oxydianiline) polyamic acid (as a polar GPE) and ethylene-vinyl acetate copolymer (EVA) containing 12 wt% vinyl acetate repeating unit (as a less polar GPE). The strong affinity of polyamic acid for $LiCoO_2$ allows the resulting PI coating layer to present a highly-continuous surface film of nanometer thickness. On the other hand, the less polar EVA coating layer is poorly deposited onto the $LiCoO_2$, resulting in a locally agglomerated morphology with relatively high thickness. Based on the characterization of GPE coating layers, their structural difference on the electrochemical performance and thermal stability of high-voltage (herein, 4.4 V) $LiCoO_2$ is thoroughly investigated. In comparison to the EVA coating layer, the PI coating layer is effective in preventing the direct exposure of $LiCoO_2$ to liquid electrolyte, which thus plays a viable role in improving the high-voltage cell performance and mitigating the interfacial exothermic reaction between the charged $LiCoO_2$ and liquid electrolytes.

A Study on the Estimation of Corrosion Protection Performance of Concrete Containing Ground Granulated Blast-Furnace Slag for Massive Coastal Structures (매시브한 해양구조물 적용을 위한 고로슬래그 혼입 콘크리트의 방청성능 평가에 관한 연구)

  • Yoo, Jae-Kang;Kim, Dong-Suk;Park, Sang-Joon;Won, Chul;Lee, Sang-Soo
    • Proceedings of the Korean Institute of Building Construction Conference
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    • 2002.11a
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    • pp.87-91
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    • 2002
  • This paper investigates the corrosion inhibition and the reduction of hydration heat properties of Ground Granulated Blast-Furnace Slag (GGBFS) added concrete. Since the massive civil structure is vulnerable to the thermal crack by hydration. adiabatic temperature rising tests were performed for water-binder ratios from 43.2% to 47.3%, while replacing 15% to 50% of cement with GGBFS of equal weight. Then, the corrosion protection performance was evaluated using cylindrical specimens embedded with steel reinforcement according to the combination of 3 W/B ratios and 2 levels of chloride ion quantity. The corrosion area of the embedded steel ban was determined using the high pressure steam curing method specified in KS F 2561. The test results showed that the replacement of GGBFS was effective in reducing the hydration heat. The corrosion area of the embedded steel ban decreased as the replacement of GGBFS increased. However, the corrosion area of the steel bar was proportional to the autoclave cycle and the chloride ion quantity. Among the tested specimens, compressive strength, reduction of hydration heat, and corrosion inhibition performance were excellent when 50% of cement was replaced with GGBFS of equal weight.

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