• Proceedings of the Korean Society of Precision Engineering Conference
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• 2006.05a
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• pp.435-436
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• 2006

This study focused on the introduction of the self healing technique for polymeric composites and evaluated the healing efficiency by the use of the interlaminar toughness fracture test. The DCPD (dicyclopentadiene) and ENB (5-ethylidene-2-norbornene) were used for the healing agent and the Grubbs' catalyst was used for the catalyst. According to the results, healing efficiency was found to be 37.9%, 22.3%, 26.3%, 22.8%, 30.8%, 30.8%, 33.0%, 33.4% for mode II fraction of 0%, 20%, 35%, 50%, 65%, 80%, 90%, 100%, respectively.

• 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 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.

• Elastomers and Composites
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• v.14 no.3
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• pp.161-168
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• 1979

이 논문(論文)의 목적(目的)은 열적안정성(熱的安定性) 및 내노화성면(耐老化性面)에 있어서 디엔제3성분단위체(第三成分單位體)(diene termonomer)의 각각(各各)의 종류(種類)가 EPDM의 중합체(重合體)의 성질(性質)에 미치는 효과(效果)를 구명(究明)하는데 있다. 제3성분단위체(第三成分單位體) 5종(種)으로 각각(各各) 다음과 같다. 즉, ethylidene norbonene(ENB), butadiene(BD), dicyclopentadiene(DCPD), methyltetrahydroindene (MTHI) 및 1,4-hexadiene(HD)이다. 이들을 써서 만든 각각(各各)의 EPDM은 동(同)몰의 불포화도(不飽和度)로 만들어졌다. 또한 가황계(加黃系)는 동일(同一)한 황/촉진제계(黃/促進劑系)를 사용(使用)하였다. ENB-EPDM이 순(純)고무배합체(配合體) 및 충전제함유배합체(充塡劑含有配合體)의 가황(加黃)에 있어서 모두 함께 가장 빠른 가황속도(加黃速度)를 보였다. HD-EPDM은 순(純)고무배합체(配合體)에서 가황속도(加黃速度)가 가장느렸으나 충전제함유배합물(充塡劑含有配合物)에서는 DCPD-EPDM보다는 발랐다. BD-EPDM을 제외(除外)한 이들 중합체(重合禮)는 거의 같은 초기가교밀도(初期架橋密度)를 갖는다. 가교밀도(架橋密度) 및 가교형(架橋型)을 분석(分析)하여 보면 BD-EPDM 쇄(鎖)에서 부타디엔 단위(單位)는 블럭을 이루고 있다. 또한 HD-EPDM은 순(純)고무가황체(加黃體) 및 충전제배합가황체(充塡劑配合加黃體)에 있어서 원가교결합(原架橋結合)의 50%가 monosulfide의 구조(構造)를 가지고있다. 이외(外)의 4종(四種)의 EPDM 폴리머는 보다 낮은 monosulfide구조를 가진다. $177^{\circ}C(350^{\circ}F)$의 노화온도(老化溫度)에서 ENB 및 HD폴리머는 약(約) 65% monosulfide 가교(架橋) 및 거의 동일(同一)한 파괴에너지값$(E_b)$을 가진다. 그러나 1,4HD의 원가교(原架橋)의 monosulfide 구조함량(含量)이 보다 높다고 해서 그의 내노화성(耐老化性)이 다른 폴리머보다 더 좋다고는 생각되지 않는다. DCPD는 $177^{\circ}C(350^{\circ}F)$의 노화온도(老化溫度)에서 똑같은 monosulfide가교(架橋)를 가지나 노화온도(老化溫度)가 $259^{\circ}C(500^{\circ}F)$로 높아짐에 따라 monosulfide 함량(含量)도 증가(增加)한다. $550^{\circ}F(287.7^{\circ}C)$의 노화온도(老化溫度)에서는 EPDM폴리머의 모든 가교(架橋)가 monosulfide구조가 되나 전가교밀도(全架橋密度) 및 $E_b$ (신장률(伸長率), 절단시(切斷時)의)는 대단(大端)히 낮은 것으로 나타나는데 이것은 산화(酸化)에 의한 노화(劣化)에 기인(基因)되는 것으로 보인다. 질소기류(窒素氣流)속에서의 TGA의 분석결과(分析結果)를 보면 EPDM 가황체(加黃體)는 $800\sim935^{\circ}F(427\sim502^{\circ}C)$의 온도범위(溫度範圍)에서 분해(分解)되며 공기중(空氣中)에서는 $750\sim935^{\circ}F$ 범위(範圍)에서 분해(分解)한다.

• 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.