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      • KCI등재

        Experimental Study on the Preparation of MA@PS@Fe3O4 Phase Change Microcapsules to Inhibit the Development of Electric Branches in Epoxy Resin Cured Compounds

        Liu Qian,Du Bin,Qi Wei,Mai Yuxiang,Zhao Yushun,Chen Nanqing 대한금속·재료학회 2022 ELECTRONIC MATERIALS LETTERS Vol.18 No.5

        Development of electric branches caused by partial discharge leads to degradation in the performance of epoxy resin insulation materials, which seriously threatens the safe and stable operation of power equipment. In this study, n-tetradecanol (MA)@polystyrene microsphere (PS)@Fe3O4 core–shell phase change microcapsules were designed and prepared. Doping 0.1 wt% phase change microcapsular material into the epoxy resin cured compound inhibited the development of electric branches. SEM and EDS tests showed that the phase-change microcapsules had monodisperse spherical core–shell structures with an MA encapsulation rate of 24.73% and excellent phase-change thermal storage capacity. Electric field simulations revealed that Fe3O4 nanoparticles in the microcapsule shell enhanced the local field strength of the cured epoxy resin and induced the development of electric branches toward the interior of the microcapsule. Moreover, doping of microcapsules into the epoxy resin significantly slowed the rate of temperature rise and thus inhibited further development of electric branches in epoxy resin cured products. In comparison with the epoxy resin cured without microcapsules, it was found that the longitudinal and transverse lengths of electric branches were reduced by 56.6% and 69.1%, respectively, in the epoxy resin cured with 0.1 wt% MA@PS@Fe3O4 microcapsules, and the electric branch initiation field strength was increased from 0.57 to 0.68 kV/mm. This indicated that MA@PS@Fe3O4 microcapsules significantly improved the electrical branch resistance of epoxy resin cured products, and this provides a new approach for extensive applications of epoxy resin insulation materials and safe and stable operation of power equipment.

      • KCI등재

        결정성 바이페닐 에폭시 합성 및 경화 거동 연구

        최봉구,최호경,최재현,최중소 한국화학공학회 2020 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.58 No.1

        The basic catalyst 1-benzyl-3-methyl-imidazolium hexafluoroantimonate (BMH) was synthesized and analyzed by FT-IR and 1H-NMR. A crystalized biphenyl-based epoxy was synthesized by using tetramethyl biphenol (TMBP) and epichlorohdrine. In order to consider the curing tendency of the synthesized BMH, the mass ratio was changed to 0.5, 1.0, 2.0 wt.% under heated conditions and the curing tendency was analyzed by differential scanning calorimeter (DSC). As a result, the BMH catalyst showed a fast curing result in the stepwise heating process of the biphenol-A epoxy and the cationic polymer. From these results, the BMH catalyst showed excellent thermal stability as a potential heat curing catalyst. In addition, we considered the application possibility of epoxy molding compound (EMC) which required a skeleton structure and a high heat resistance because the synthesized biphenyl epoxy had a characteristic of rapidly lowering viscosity at a constant temperature and a rigid skeleton structure of biphenol. As a result, it was confirmed that the TMBP-based epoxy developed in this study was composed of a crystalline structure, and a curing reaction was observed with a Novolac resin at a high temperature. In the presence of a catalyst, a curing reaction was observed around 150 oC and thus TMBP-based epoxy was successfully applied as a raw material of EMC. n-Methylimidazole, acetonitrile, benzylbromide 및 sodiumhexafluoroantimonate를 이용하여 염기성 촉매 1-benzyle- 3-mehyl-imidazolium hexafluoroantimonate (BMH)를 합성하고, tetramethyl biphenol (TMBP)과 epichlorohydrine을 이용하여 결정성 바이페닐 에폭시를 합성하여 FT-IR과 1H-NMR으로 구조를 분석하였다. 합성한 촉매 BMH의 경화 거동을 고찰하기 위하여 0 oC에서 250 oC까지 5 oC/min의 속도로 승온시키면서 에폭시 수지에 대하여 BMH의 질량비를0.5, 1.0, 2.0 wt.%로 변화시켜 시차주사 열량계(differential scanning calorimeter, DSC)로 분석하였다. 그 결과, BMH 촉매는 비스페놀 A형 에폭시와 양이온 중합체의 단계적 가열과정에서 빠른 경화 특성을 보였다. 또한 합성한 바이페닐 에폭시는 일정한 온도에서 급격히 점도가 낮아지는 특성과 바이페놀의 강직한 골격구조를 가지는 특성을 가지고있기 때문에 결정성 구조 및 고내열성을 요구하는 반도체용 봉지재료의 대표격인 epoxy molding compound (EMC)의원료로서의 적용 가능성을 고찰하였다. 그 결과, 본 연구에서 개발한 바이페닐 에폭시는 결정성 구조로 이루어진 것을확인하였으며, 경화제로 페놀 노볼락수지와 고온에서의 경화반응 시, BMH 촉매 존재 시에는 150 oC 근처에서 경화반응이 관찰되어 EMC의 원료로 사용될 수 있음을 확인하였다.

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