以石墨烯改質黏土與無機層材奈米混成於 酚醛環氧樹脂複合材料之難燃性研究

Study on the Flammability of Novolac Epoxy Resin／Graphene Modified Clays and Layered Double Hydroxide Nanocomposites

麥豪麟(Hao-Lin Mai)

指導教授 ： 蔡宗燕

中原大學/理學院/化學研究所/碩士(2018年)

https://doi.org/10.6840/cycu201800597

摘要

在本研究中首先針對石墨烯進行有機官能化改質使其帶有四級銨鹽或羧酸根官能基，再以水中之懸浮分散性、拉曼光譜及熱重分析儀檢測了解有機官能化是否成功。接著將已有機官能化石墨烯、天然黏土、層狀雙氫氧化合物與改質劑進行有機改質，利用廣角X射線繞射分析儀、傅立葉轉換遠紅外光譜儀、掃描式電子顯微鏡和熱重分析儀鑑定黏土或鎂鋁層狀雙氫氧化合物改質前後的層間距變化，改質劑進入黏土或鎂鋁層狀雙氫氧化合物的比例及其熱穩定性與表面型態。將有機官能化石墨烯改質之黏土或鎂鋁層狀雙氫氧化合物分別與酚醛環氧樹脂進行交聯反應，製備成奈米級複合材料並藉由廣角X射線繞射分析儀、穿透式電子顯微鏡檢測其分散型態，以熱重分析儀試測其耐熱性質，以動態分析儀檢測其儲存模數玻璃轉移溫度的變化，最後以限氧指數儀檢測其難燃性質，再分別添加機官能化石墨烯改質之黏土與層狀雙氫氧化合物後LOI值從純的酚醛環氧樹脂21.10分別提升到29.80、31.50與32.50。並將製備出來的配方應用於銅箔基板的製作，藉此探討銅箔基板之各項性質變化、UL 94與圓錐測量儀的阻燃性。檢測結果以3 wt% MgAl-DMSI-OGC之複合材料難燃效果較佳，並且以此組成配製成之銅箔基板可符合各項數值測試，同時UL 94達到V-1耐燃等級，另外輔以圓錐測量儀的檢測，其最大熱釋放速率從350.2 kW/m2下降到263.3 kW/m2、總熱釋放量從10.42 MJ/m2下降到7.18 MJ/m2與引燃時間從42秒延長到59秒。

關鍵字

天然黏土 ； 層狀雙氫氧化合物 ； 石墨烯 ； 酚醛環氧樹脂

並列摘要

In this study, graphene was organofunctionalized by quaternary ammonium or carboxylate functional groups. After the functionalization of graphene, which was successfully confirmed by Raman spectroscopy, and thermogravimetric analysis. Furthermore, the modified graphene was applied to modified layered materials (naturals clay or MgAl LDHs). These modified layered materials were examined by wide Angle X-ray diffraction (WXRD), Fourier Transform Infrared spectrometers (FT-IR), Scanning Electron Microscope (SEM), and Thermo Gravimetric Analysis (TGA) to identify the interlayer spacing, functionalgroups of nanofillers,clispersion morphology, and intercalated amount of modified, respectively.
Preparation of modified nanfillers was applied to the flame retardant for Novolac epoxy resin／graphene modified clays / MgAl LDHs nanocomposites. The dispersion morphology of nanocomposites were examined by WXRD, Transmission electron microscope (TEM). Thermal mechanical properties investigated by using TGA and Dynamic Mechanical Spectrometer (DMA). Furthermore, limiting oxygen index (LOI) test were applied to evaluate the flammability of nanocomposites. The LOI value increased pure novolac epoxy resin and novolac epoxy resin nanocomposites from 21.10 to 29.80, 31.50 and 32.50, respectively. Among these Composition of nanocomposites, the best propenties of nanocomposites to make copper clad laminate (CCL) and check the flammability properties by UL 94, The peak heat release rate (PHRR) and total heat release(THR) and time of ignition (Tign) measured by cone calorimeter. In addition, with the detection of the cone measuring instrument, the peak heat release rate of epoxy nanocomposites decreased from 350.2 kW/m2 to 263.3 kW/m2, and the total heat release decreased from 10.42 MJ/m2 to 7.18 MJ/m2 time of ignition decreased from 42 second to 59 second.3wt% MgAl-DMSI-OGC-Epoxy nanocomposites have shown the best flammability.

並列關鍵字

Novolac Epoxy Resin ； Graphene ； Clays ； Layered Double Hydroxide ； Nanocomposites

參考文獻

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