POSS/粘土/多壁碳纳米管杂化碳纳米纸基复合材料防火性研究

doi:10.3724/SP.J.1077.2014.13500

摘要/Abstract

摘要：

多壁碳纳米管(MWCNTs)、粘土和多面齐聚半硅氧烷(POSS)组成的杂化碳纳米纸是通过碳纳米管巴基纸制备工艺制备而成, 碳纳米纸可做为表面防火层与聚合物基复合材料共固化成型。利用场发射扫描电镜(FESEM)和BJH法分别对碳纳米纸和杂化碳纳米纸微观结构和平均孔径分布进行表征。利用锥形量热仪在热辐射功率50 kW/m²条件下分析外贴碳纳米纸复合材料及复合材料对比样的防火特性。燃烧实验结果表明: 碳纳米纸和杂化碳纳米纸作为防火层的复合材料的峰值热释放速率(PHRR)与复合材料对比样相比分别下降20.2%和35%, 同时CO释放量和烟释放量也明显降低。通过FESEM研究表明燃烧实验后外贴杂化碳纳米纸复合材料的燃烧残余物表面形成了一层致密的积炭物结构, 防火阻燃性能明显提高。

关键词: 碳纳米纸, 粘土, 多面齐聚半硅氧烷(POSS), 锥形量热仪, 防火性

Abstract:

A hybrid buckypaper consisting of multi-walled carbon nanotubes (MWCNTs), clay and polyhedral oligomeric silsesquioxane(POSS) was fabricated through vacuum filtration method. The as-prepared buckypaper (or hybrid buckypaper) can be incorporated onto the surface of fiber reinforced polymer composite as surface fire shields. The morphology and pore size distribution of the MWCNTs buckypaper were characterized with field emission scanning electron microscope (FESEM) and Barret-Joyner-Halenda(BJH) method. The fire retardant performance of composite laminates coated with (or without) the buckypaper was thoroughly evaluated by cone calorimeter testing at a radiant heat flux of 50 kW/m². Compared with the contral composite, the peak heat release rate (PHRR) of composite surface coated MWCNTs buckypaper or the hybrid buckypaper reduced more than 20.2% and 35%, respectively. The CO production rate and the smoke production rate reduced obviously. The formation of compact char material can be observed on the surface of the composite residues and analyzed by FESEM, the fire retardant property of composite can be improved by surface coated hybrid buckypaper.

Key words: buckypaper, POSS, clay, cone calorimeter, fire retardancy

中图分类号:

TB33
TB34

卢少微, 曾宪君, 张春旭, 王继杰, 聂鹏. POSS/粘土/多壁碳纳米管杂化碳纳米纸基复合材料防火性研究[J]. 无机材料学报, 2014, 29(6): 589-593.

LU Shao-Wei, ZENG Xian-Jun, ZHANG Chun-Xu, WANG Ji-Jie, NIE Peng. Fire Retardancy of Fiber Reinforced Polymer Composites Coated with POSS/Clay/MWCNTs Hybrid Buckypaper[J]. Journal of Inorganic Materials, 2014, 29(6): 589-593.

图/表 9

图1 碳纳米纸和外贴碳纳米纸复合材料照片

Fig. 1 Photographs of buckpaper and hybrid buckypaper (a) Buckpaper; (b) Hybrid buckypaper; (c) Composite surface coated buckypaper; (d) Composite surface coated hybrid buckypaper

图2 与复合材料共固化后碳纳米纸(a)和杂化碳纳米纸(b)的FESEM照片

Fig. 2 FESEM images of buckypaper (a) and hybrid buckypaper (b) co-cured with composite

表1 不同复合材料试样的组成

Table 1 Composition of composites

Samples	Contents/wt%
Samples	GF	Resin	Buckypaper
Control	60	40	0
GF/BP	57.2	39.7	2.1
GF/BP/POSS+Clay	53.8	40.0	2.2

图3 碳纳米纸孔径分布图

Fig. 3 Distribution of pore size diameter for buckypaper

图4 复合材料的热释放速率(A)和有效燃烧热曲线(B)

Fig. 4 Comparison of heat release rate curves (A) and effective heat of combustion curve (B) for composite sample

表2 复合材料锥形量热仪数据

Table 2 Cone calorimetric data for laminate composite samples.

Sample	TTI/s	Peak HRR<br/>/(kW•m^-2)	Time to peak HRR/s	Total heat release /(kW•m^-2)	Average HRR<br/>/(kW•m^-2)	Total smoke release<br/>/(m²•m^-2)	Peak CO production rate<br/>/(kg•kg^-1)	Average EHC<br/>/(MJ•kg^-1)
Control	52	113.2	85	11.1	38.6	254.4	15.7	19.0
CF/BP	60	90.3	90	10.1	33.9	244.7	8.6	18.4
CF/BP/Clay+POSS	62	73.6	110	7.3	25.3	229.9	0.74	17.4

图5 复合材料试样的CO释放速率曲线(A)与烟生成速率曲线(B)对比曲线

Fig. 5 Comparison of CO production rate (A) and smoke production rate cures (B) for composite samples

图6 燃烧实验前碳纳米纸(a)和杂化碳纳米纸(b)的FESEM照片

Fig. 6 FESEM images of buckypaper (a) and hybrid buckypaper (b) before zone test

图7 燃烧实验后外贴碳纳米纸(a)和杂化碳纳米纸(b)的FESEM照片和残炭照片(插图)

Fig. 7 FESEM images and optical pictures (Insets) of char materials of composites surface coated with buckypaper (a) and hybrid buckypaper (b) after cone test

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