• Composites Research
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• v.17 no.4
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• pp.40-46
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• 2004

A single lap shear test was used to investigate the effects of the ratio of a catalyst to a self-healing agent and curing temperature on the bond performance of autonomic polymer composites. DCPD (dicyclopentadiene), ENB (5-ethylidene-2-norbornene), and their mixture were used as self-healing agents and bis(triclohexylphosphine) benzyllidine ruthenium (IV) dichloride Grubbs' catalyst was used as a catalyst. During the experiments, the catalyst ratios of 1.0wt% and 0.5wt% were applied to DCPD, the catalyst ratio of 0.lwt% was applied to ENB, and the catalyst ratio of 0.5wt% was applied to the mixtutes of DPCD and ENB. In addition, the curing temperatures of $25^{\circ}C$, $60{\circ}C$, and $80^{\circ}C$ were considered. According to the results, the higher catalyst ratio and the longer curing time were required to obtain more stabilized bond shear strength of DCPD. ENB with a lower catalyst ratio was cured faster than DCPD. Unlike DCPD, ENB stabilized after a steady fall from its peak as the curing time increased. Moreover, the mixtures of DCPD and ENB revealed similar curing behavior to ENB, but the increase in mixture ratio of ENB to DCPD caused curing process to be faster. Also the increase in curing temperature caused the bond shear strength to be higher and the curing time to be quicker.

• Composites Research
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• v.28 no.6
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• pp.395-401
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• 2015

This study investigated the thermal stability of Grubbs' catalyst and its reactivity with self-healing agents for self-healing damage repair. Four types of Grubbs' catalyst supplied by manufacturers were considered and each catalyst was tested in as-received and grinded conditions. Four types of self-healing agents were prepared by varying the mixing ratio of dicyclopentadiene (DCPD) and 5-ethylidene-2-norbonene (ENB). Heat flows as a function of temperature were measured through a differential scanning calorimetry (DSC) to determine the thermal stability of catalysts. Reaction heats of self-healing agents with the catalyst were measured to evaluate the reactivity of the catalyst. For this evaluation, Fluka Chemika Grubbs' catalyst was used based on the maximum temperature and the time to reach the maximum temperature. According to the results, catalysts had different shapes depending on the manufacturer and the results showed that the smaller the size of the catalyst the higher the reactivity with self-healing agents. As the ENB ratio in self-healing agents increased, the maximum temperature increased, and the time to reach the maximum temperature decreased. As the amount of the catalyst increased, the maximum temperature increased, and the time to reach the maximum temperature decreased. Considering the thermal stability of the catalyst and its reactivity with the self-healing agent, combination of 0.5 wt% catalyst and the D3E1 self-healing agent was optimal for self-healing damage repair. Finally, as the thermal decomposition may occur depending on the environmental temperature, the catalyst must not be exposed to temperature higher than that is necessary to maintain the thermal stability of the catalyst.

• Proceedings of the Korean Society of Propulsion Engineers Conference
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• 2006.05a
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• pp.202-205
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• 2006

Some advanced nations have already developed and utilized high performance carbocyclic compounds as liquid fuel components. The common point of these compounds includes polycycles. We synthesized some promising compounds which include multiplex ring form. According to three kinds of cyclopropanation method, we could synthesize five target materials and measure their physical properties.

• 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.

• Bulletin of the Korean Chemical Society
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• v.33 no.12
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• pp.4131-4136
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• 2012

Several palladium complexes containing ${\beta}$-ketoiminate and ${\beta}$-diketiminate ligands successfully produced poly(DCPD) possibly via vinyl addition. It was found that catalysts with ${\beta}$-diketiminate ligands containing bulkier aryl substituents showed the highest activity in the presence of MAO as a cocatalyst. Purity of DCPD is quite essential for the higher activity and small amount of organic solvent such as $CH_2Cl_2$ and toluene is required to reduce the viscosity of the reactant mixture for the higher activity. $^1H$ NMR spectra of produced polymers with N,N-dimethylanilinium tetra(pentafluorophenyl)borate (N,N-DAPFAr"$_4$) show that 5,6-double bond of DCPD is removed with 2,3-double bond remaining. Produced poly(DCPD) with MAO cocatalyst is quite rigid and insoluble in common organic solvents but rather brittle.

• Proceedings of the Korea Society of Environmental Toocicology Conference
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• 1996.12a
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• pp.63-63
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• 1996

We performed chromosomal aberration assay in Chinese Hamster Lung (CHL) cells in vitro to evaluate theclastogenicity of 11 synthetic chemicals which were listed in Toxicity Evaluation Program of Ministry of Environment of Republic of Korea in 1996. All of the chemicals were carried out MTT assay to determine the 50% cell growth inhibition concentration. All compounds were tested with and without metabolic activation system. Benzoyl chloride revealed positive result at $43\;\mu\textrm{g}/m{\ell}$ in the presence of metabolic activation system, and at 30.8, 61.5 and $123\;\mu\textrm{g}/m{\ell}$ in the absence of metabolic activation system. And p-phenoxy ethanol was observed as positive with the metabolic activation system, but negative without metabolic activation system. Especially 2-propyn-l-ol showed high frequency of pulverization and showed critical difference of cytotoxicity between with and without S9 mixture. Pulverizatiuon is not included in the frequency of structural aberration in our criteria. Dicyclopentadiene, methacrylic acid, aa-dimethylbenzyl hydroperoxide, benzylbutyl phthalate, and p-chlorophenal were revealed negative results.esults.

• Composites Research
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• v.31 no.2
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• pp.57-62
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• 2018

Interfacial and mechanical properties of neat and two sizing agents coated glass fiber (GF)/polydicyclopentadiene (p-DCPD) composites were evaluated at room and low temperatures, $25^{\circ}C$ and $-20^{\circ}C$. Sizing agents of GFs were extracted using acetone and compared via FT-IR. Surface energy and work of adhesion between GFs and p-DCPD were calculated by dynamic contact angle measurement. Mechanical properties of different GFs were determined using single fiber tensile test and interfacial properties of single GF reinforced DCPD strip were determined using cyclic loading tensile test. Mechanical properties of GFs/p-DCPD composites at room and low temperatures were determined using tensile, compressive, and Izod impact tests. Interfacial and mechanical properties were different with sizing agents of GFs and the optimized condition of sizing agent was found.

• Composites Research
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• v.30 no.2
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• pp.138-144
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• 2017

Damage sensing of polymer composite films consisting of poly(dicyclopentadiene) p-DCPD and carbon nanotube (CNT) was studied experimentally. Only up to 1st ring-opening polymerization occurred with the addition of CNT, which made the modified film electrically conductive, while interfering with polymerization. The interfacial adhesion of composite films with varying CNT concentration was evaluated by measuring the wettability using the static contact angle method. 0.5 wt% CNT/p-DCPD was determined to be the optimal condition via electrical dispersion method and tensile test. Dynamic fatigue test was conducted to evaluate the durability of the films by measuring the change in electrical resistance. For the initial three cycles, the change in electrical resistance pattern was similar to the tensile stress-strain curve. The CNT/p-DCPD film was attached to an epoxy matrix to demonstrate its utilization as a sensor for fracture behavior. At the onset of epoxy fracture, electrical resistance showed a drastic increase, which indicated adhesive fracture between sensor and matrix. It leads to prediction of crack and fracture of matrix.

• Composites Research
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• v.29 no.5
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• pp.282-287
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• 2016

p-DCPD (poly dicyclopentadiene) is the resin that the versatile mechanical properties can be changeable via the control of inner monomer and catalysts. In this work, to improve the strength of composites, surface treated MGF (milled glass fiber) was used as an reinforcement in p-DCPD by molybdenum (Mo) catalyst matrix. The optimum concentration of surface treatment was obtained and the cohesion of MGF themselves increased with concentration. In case of 0.2 wt% silane concentration, the maximized mechanical properties of MGF/p-DCPD composite exhibited because of minimized MGF cohesion. When butyl silane showing minimizing cohesion was used as the optimized alkyl length, high tensile and flexure strength exhibited due to the steric hindrance effect among MGFs. Mechanical and their fractured surfaces of MGF/p-DCPD composites was compared for 4 different chemical functional groups. Norbornene functional groups containing similar chemical structure to DCPD matrix exhibited higher interfacial adhesion between MGFs and DCPD matrix.

• Composites Research
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• v.16 no.2
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• pp.54-61
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• 2003

In this study, manufacturing process for microcapsules with the self-healing agent was introduced and the characteristics of microcapsules manufactured by varying with various manufacturing process variables were evaluated through a particle size analyzer, an optical microscope, and a TGA. Urea-formaldehyde resin was used for the thin wall of microcapsules and DCPD (dicyclopentadiene) was used for the self-healing agent. The various manufacturing process variables, such as (1) 24hr, 40hr, 48hr, 60hr of the solution time of the EMA copolymer, (2) pH3.5, pH4.0, pH4.5 of the hydrogen ion concentration of the emulsified solution, (3) 400rpm, 500rpm, 600rpm, 1000rpm of the agitation speed of the emulsified solution, (4) $50^{\circ}$, $55^{\circ}$, $60^{\circ}$ of the reaction temperature of the emulsified solution, were considered. According to the results, the particle size distribution of microcapsules was affected on the agitation speed, and the thermal stability of microcapsules was influenced by the solution time of the EMA copolymer, the hydrogen ion concentration, and the reaction temperature of the emulsified solution. Therefore, suitable manufacturing process variables should be applied to obtain thermally stable microcapsules capable of containing the healing agent capable until the thin wall of microcapsules were to be burned.