聚合物/氧化石墨烯納米復(fù)合材料燃燒性能研究

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摘要
氧化石墨烯是近幾年來(lái)發(fā)展起來(lái)的一種新型二維無(wú)機(jī)納米材料，自從其發(fā)現(xiàn)以來(lái)，氧化石墨烯在化學(xué)、物理、材料、電子等各個(gè)領(lǐng)域顯示了廣闊的應(yīng)用前景。尤其是它們極高的機(jī)械強(qiáng)度、出色的導(dǎo)電和導(dǎo)熱性能，以及豐富的原料來(lái)源，使其能作為一種理想的無(wú)機(jī)納米填料來(lái)制備聚合物復(fù)合材料。但是目前為止，氧化石墨烯材料的大規(guī)模制備并應(yīng)用于火災(zāi)安全方面，以及如何將氧化石墨烯均勻地分散到聚合物基體中并且優(yōu)化氧化石墨烯與聚合物基體之間的界面作用力一直是科學(xué)界及工業(yè)界尚待解決的難題。本學(xué)位論文圍繞著這些問(wèn)題進(jìn)行了一系列研究。具體研究?jī)?nèi)容及結(jié)果如下：
1、采用改進(jìn)的Hummers法制備氧化石墨烯;
2、采用浸滯、包裹和烘干等步驟制備氧化石墨烯包裹海綿納米復(fù)合材料，并研究其阻燃性能。
2、采用共混法制備PP/氧化石墨烯納米物復(fù)合材料，并研究其阻燃性能。
實(shí)驗(yàn)結(jié)果表明，采用改進(jìn)的Hummers法制備了石墨烯片層堆積厚度約為5-6nm，為5-6層的石墨烯。燃燒實(shí)驗(yàn)結(jié)果表明，隨著包裹海綿的氧化石墨烯濃度的提升，其阻燃性能改善越明顯。當(dāng)采用0.003g/mL對(duì)海綿進(jìn)行浸泡包裹得到的石墨烯包裹海綿納米復(fù)合材料在阻燃方面得到明顯提高，但當(dāng)濃度高于0.003g/mL后，對(duì)海綿的阻燃性能影響較小。另外，對(duì)PP/氧化石墨烯聚合物復(fù)合材料的垂直燃燒測(cè)試和極限氧指數(shù)測(cè)試都發(fā)現(xiàn)，氧化石墨烯的引入對(duì)其阻燃性能的提高具有促進(jìn)作用。

關(guān)鍵詞：氧化石墨烯；海綿；包裹；納米復(fù)合材料；阻燃性能


ABSTRACT
Graphene oxide is novel two-dimensional inorganic nano-materials developed recently, it has great promise applications in the fields of chemistry, physics, material science, electronics, and so on, since its first successful fabrication. Graphene oxide is ideal inorganic nanofillers for reinforcement of polymer composite materials because of its ultrahigh mechanical property, excellent electrical and thermal conductivity, and abundant resources (graphite). However, they are still obstacles to be resolved in both academia and industry, including the mass preparation of graphene oxide, the applications into fire safety and the homogeneous incorporation of graphene oxide into polymer matrix and optimizing the interfacial interactions between them. With the aim of addressing these problems, numerous researches have been done in this thesis. The details of research are listed as follows:
1. Graphene oxide was prepared by a modified Hummers method.
2. Graphene oxide coating sponges nanocomposites were preparated by immersion, coating and drying processes, and their flame retardant properties were investigated.
3. GO/PP nanocomposites were prepared by melt blending method, and their fire retardant properties were studied.
From the results, the average stacking height of sheet Lc (the crystalline thickness of the (002) facet), was estimated to be ~5-6 nm, corresponding to no more than 5-6 graphene layers. The experiment results of combustion show that the fire retardant properties were improve obviously with increasing concentration of graphene oxide. When the concentration of graphene oxide was 0.003 g/mL, the fire retardant properties of graphene oxide coating sponge nanocomposites were increased remarkably. However, when the concentration reaches to a specific level, the effect of graphene oxide could be neglected for the combustion properties. In addition, the GO plays a positive role in the enhancement of the fire retardant properties of PP /GO nanocomposites from both UL-94 and LOI.

KEYWORDS: graphene oxide; sponges; coating; nanocomposites; fire retardant properties


目 錄
摘要 v
ABSTRACT vi
縮略詞對(duì)照表 vii
第一章 緒論 1
1.1 引言 1
1.2 無(wú)鹵阻燃技術(shù)的現(xiàn)狀和研究進(jìn)展 1
1.2.1 傳統(tǒng)膨脹阻燃體系 2
1.2.2 新型膨脹阻燃體系 3
1.2.3 協(xié)同阻燃技術(shù) 4
1.2.4 微膠囊化阻燃技術(shù) 6
1.2.5 納米復(fù)合阻燃技術(shù) 7
1.3 氧化石墨烯的制備及聚合物/氧化石墨烯納米復(fù)合材料阻燃性能研究 9
1.3.1 氧化石墨烯的制備方法 10
1.3.2 氧化石墨烯的結(jié)構(gòu) 11
1.3.3 氧化石墨烯的性質(zhì) 12
1.3.4 氧化石墨烯聚合物納米復(fù)合材料的制備方法 13
1.3.5 聚合物阻燃性能和阻燃機(jī)理研究 14
1.4 研究目標(biāo)及意義 16
1.5 研究思路與研究?jī)?nèi)容 17
1.5.1 研究思路 17
1.5.2 研究?jī)?nèi)容 17
第二章 氧化石墨烯及其聚合物納米復(fù)合材料的制備與阻燃性能測(cè)試 19
2.1 引言 19
2.2 實(shí)驗(yàn)中所用藥品和儀器 19
2.3實(shí)驗(yàn)操作步驟及過(guò)程 21
2.3.1 氧化石墨烯的制備 21
2.3.2 氧化石墨烯的剝離 24
2.3.3 氧化石墨烯包裹海綿納米復(fù)合材料的制備和燃燒實(shí)驗(yàn) 25
2.3.4 PP/氧化石墨烯納米復(fù)合材料的制備及燃燒性能測(cè)試 26
2.4 氧化石墨烯表征及其復(fù)合材料阻燃性能測(cè)試方法 28
2.4.1掃描電鏡（SEM）形貌觀察 28
2.4.2　X-射線衍射分析 28
2.4.3透射電鏡(TEM)形貌觀察 29
2.4.4拉曼光譜儀測(cè)試 29
2.4.5極限氧指數(shù)測(cè)試（LOI） 29
2.4.6垂直燃燒測(cè)試（UL-94） 29
第三章 氧化石墨烯及其聚合物納米復(fù)合材料阻燃性能研究 31
3.1氧化石墨烯的表征 31
3.1.1 石墨、氧化石墨烯的XRD測(cè)試結(jié)果 31
3.1.2石墨、氧化石墨烯的拉曼圖譜結(jié)果和分析 32
3.1.3氧化石墨烯的掃描電鏡照片分析 34
3.1.4氧化石墨烯洗滌前后透射電鏡照片分析 34
3.2氧化石墨烯包裹海綿納米復(fù)合材料..