以石墨烯改質黏土奈米混成於酚醛環氧樹脂複合材料之阻燃性研究

Study on the Flammability of Novolac Epoxy Resin／Graphene－Intercalated－Modified Clays Nanocomposites

黃賢平(Hsien-Ping Huang)

指導教授 ： 蔡宗燕

中原大學/理學院/奈米科技碩士學位學程/碩士(2015年)

https://doi.org/10.6840/cycu201500777

摘要

本研究以不同層數的石墨烯作為改質劑之一，分別與天然黏土作為分散載體與補強材，期望同時利用黏土層間的結晶水與氫氧基受熱脫水，降低熱的釋放量，氣化的水蒸氣可以降低氧含量，天然黏土與石墨烯的片狀結構阻隔熱傳與氧氣的提供，另外石墨烯豐富的雙鍵在燃燒時產生自由基可以捕捉高分子熱裂解產生的氫自由基與氫氧自由基，以達到阻燃的效果。在本研究中，將石墨烯先進行官能化，並以拉曼光譜(Raman)與熱重分析(TGA)儀檢測了解官能化前後的差異。接著將官能化石墨烯、天然黏土與改質劑進行有機改質後，利用廣角X光繞射儀(WXRD)、熱重分析儀(TGA)與紅外線光譜儀(FTIR)了解改質前後黏土的層間距變化，以及改質劑進入黏土層間中的比例。之後將改質後黏土與酚醛環氧樹脂進行交聯反應製成奈米級複合材料，藉由廣角X光繞射儀(WXRD)與穿透式電子顯微鏡驗證黏土在酚醛環氧樹脂中的分散型態，並利用熱重分析儀(TGA)與動態機械分析儀(DMA)了檢測奈米複合材料的熱裂解溫度(Td)及複材的玻璃轉移溫度(Tg)的變化。最後利用極限氧指數儀(LOI)、圓錐量熱儀(Cone calorimeter)來測試複材的耐燃性，並將效果最好的配方實際應用在銅箔基板的製程，探討各項性質的變化與UL-94的阻燃性。結果發現，3wt%CL120-PI-BEN-OGNS-300之複材其耐燃效果最佳，且製成之銅箔基板也通過各項數值測試及UL-94達到V1耐燃等級。

關鍵字

環氧樹脂 ； 銅箔基板 ； 石墨烯 ； 阻燃性

並列摘要

Functionalized inorganic layered material (clay) based on modification system composed by Benzalkonium-N-methyl pryrrolidine-graphene, were designed and fabricated in this study to synthesize novolac cured epoxy nanocomposites. Clays, as dispersed template, were modified by methyl pyridine functionalized graphene materials, such as multilayers and mono layer graphene intercalants. There are functionalized graphene materials to enhance the fire retardant of resulting nanocomposites. The functionalized graphene characterized by Raman spectroscopy, and thermo-gravimetric analysis (TGA) was applied to confirm the difference functionalities of graphene. The modified clays were characterized by wide-angle X-ray diffraction (WAXD), TGA and Fourier transform infrared spectroscopy (FTIR) to confirm the inclusion of modified agents into clay layers. The dispersion morphology of clay in the novolac cured epoxy resin was analyzed by WXRD and transmission electron microscopy (TEM). TGA and dynamic mechanical analysis (DMA) were used to measure the thermal and mechanical properties. Finally, limiting oxygen index (LOI) and cone calorimeter test were applied to evaluate the flammability of these nanocomposites. The best composites of modified clay/novolac cured epoxy nanocomposites were selected to make copper clad laminate (CCL) and discussed the properties and flammability. Consequence, 3wt% CL120-PI-BEN-OGNS-Epoxy nanocomposites has shown the best flammability. Apply this result to make the copper clad laminate which has passed the UL-94-V1 test.

並列關鍵字

Epoxy ； Copper Clad Laminate ； Graphene ； Flame retardant

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