碳纳米管/有机硅树脂吸波气凝胶及其复合材料的制备与性能

王晓岚; 柳云钊; 孔磊; 师建军; 杨云华

碳纳米管/有机硅树脂吸波气凝胶及其复合材料的制备与性能

王晓岚^{1, 2},
柳云钊^{1, 2},
孔磊^{1, 2, ,},
师建军^{1, 2},
杨云华^{1, 2}

1.
航天材料及工艺研究所, 北京 100076
2.
先进功能复合材料技术国防科技重点实验室, 北京 100076

详细信息

通讯作者:
孔磊，博士，研究员，硕士生导师，研究方向为树脂基功能复合材料　E-mail: polymz@163.com

中图分类号: TB332, TB34
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- 文章访问数: 100
- HTML全文浏览量: 54
- 被引次数: 0
出版历程
- 收稿日期: 2024-04-01
- 修回日期: 2024-05-15
- 录用日期: 2024-05-17
- 网络出版日期: 2024-06-15

Preparation and properties of carbon nanotubes/ silicon microwave absorbing aerogel and its composite

WANG Xiaolan^{1, 2},
LIU Yunzhao^{1, 2},
KONG Lei^{1, 2
, ,},
SHI Jianjun^{1, 2},
YANG Yunhua^{1, 2}

1.
Aerospace Research Institute of Materials & Processing Technology, Beijing 100076, China
2.
Science and Technology on Advanced Functional Composites Technology, Beijing 100076, China

摘要

摘要: 基于溶胶-凝胶方法，制备不同比例多壁碳纳米管改性有机硅树脂(CNT/OSR)气凝胶和针刺石英纤维增强CNT/有机硅树脂气凝胶(QF/SC)复合材料，探究CNT含量对有机硅气凝胶及其复合材料的微观结构、防热性能和吸波性能的影响规律。研究结果表明：进行物理修饰后的CNT与有机硅树脂表现出良好的相容性，构建起了微导电、导热通道；改性后树脂的热稳定性有了明显提升，当CNT的质量分数为有机硅树脂的15wt%时，T_d10提升111.1℃；QF/SC复合材料热导率在0.054~0.075 W/(m·K)之间，经600 s表面温度达1000℃的烧蚀后，最大背温为145.1℃；引入碳纳米管的QF/SC复合材料介电性能显著提高，实测8~18 GHz内反射率峰值和有效带宽分别达到−29 dB和3 GHz。该项工作有望在航空航天科学和工业领域实现新的应用。
- 有机硅树脂 /
- 碳纳米管 /
- 气凝胶 /
- 吸波 /
- 防热
Abstract: Utilizing the sol-gel method, this study presents the fabrication of carbon nanotubes/organic silicon resin (CNT/OSR) aerogels and quartz fibre-reinforced CNT/silicon (QF/SC) composites incorporating varying proportions of multi-wall carbon nanotubes. The investigation focuses on discerning the influence of CNT content on the microstructural, thermal, and wave absorption properties of silicone aerogels and their composites. Results demonstrate the favorable compatibility of modified CNT with silicone resin, facilitating the establishment of micro-conductive and thermal conductive pathways. Remarkable enhancement in thermal stability of the modified resin is observed, notably with a 111.1℃ increase in T_d10 when the CNT mass fraction constitutes 15wt% of the silicone resin. Moreover, the thermal conductivity of QF/SC composites spans from 0.054 to 0.075 W/(m·K), with a maximum rear temperature of 145.1℃ attained after 600 s exposure at 1000℃. Furthermore, the introduction of carbon nanotubes substantially augments the dielectric properties of QF/SC composites, leading to peak reflectance and effective bandwidth measurements within the range of 8-18 GHz, registering at -29 dB and 3 GHz, respectively. This research anticipates fostering novel applications in aerospace science and industry.
- Silicone resin /
- carbon nanotubes /
- aerogel /
- microwave absorption /
- thermal protection

HTML全文

图 1 碳纳米管改性有机硅树脂(CNT/OSR)气凝胶及针刺石英纤维增强碳纳米管/有机硅树脂气凝胶(QF/SC)复合材料的制备流程示意图

Figure 1. Schematic diagram of preparation process of fabrication of carbon nanotubes/organic silicon resin (CNT/OSR) aerogel and quartz fibre-reinforced CNT/silicon (QF/SC) composite

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图 2 (a)室温静置一周后未进行改性和改性后的碳纳米管分散液；(b) QF/SC复合材料示意图

Figure 2. (a) unmodified and modified CNT dispersion after stand at room temperature for a week, (b) picture of QF/SC composites

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图 3 有机硅树脂固化前后的FTIR图谱

Figure 3. FTIR spectra of silicone resin

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图 4 (a) CNT, (b) S-0, (c) SC-2, (d) SC-5, (e) SC-10, (f) SC-15样品的微观形貌图像

Figure 4. Micro morphological images of (a) CNT, (b) S-0, (c) SC-2, (d) SC-5, (e) SC-10, (f) SC-15 samples

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图 5 不同CNT/OSR气凝胶的孔径分布图

Figure 5. Pore diameter and its distribution curves of CNT/OSR aerogels

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图 6 不同CNT/OSR气凝胶的TGA和DTG曲线

Figure 6. TGA and DTG curves of CNT/OSR aerogels

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图 7 不同QF/SC复合材料的介电常数的(a)实部、(b)虚部和(c)介电损耗正切

Figure 7. (a) Real part and (b) imaginary part of the complex permittivity and (c) dielectric loss tangents for QF/SC composites

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图 8 (a) QF/SC-2、(b) QF/SC-5、(c) QF/SC-10、(d) QF/SC-15复合材料反射损耗2 D、3 D示意图

Figure 8. Reflection loss 2 D and 3 D diagram of (a) QF/SC-2、(b) QF/SC-5、(c) QF/SC-10、(d) QF/SC-15 composites

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图 9 不同QF/SC复合材料在8 mm厚度8~18 GHz波段内的反射损耗曲线

Figure 9. Reflection loss plot of QF/SC composites at 8 mm thickness in 8~18 GHz

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图 10 碳纳米管改性有机硅气凝胶及复合材料吸波机制示意图

Figure 10. Schematic diagram of MA mechanism of carbon nanotube modified silicone aerogel

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图 11 QF/SC-5复合材料烧蚀考核表温和背温曲线

Figure 11. Surface and back temperature curves of QF/SC-5 composites during ablation test

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图 12 高温烧蚀后QF/SC-5复合材料层分布示意图与微观形貌照片

Figure 12. Distribution diagram and microstructure pictures of QF/SC-5 composites after high temperature ablation

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表 1 不同CNT含量的CNT/OSR气凝胶的性能参数

Table 1. Properties of CNT/OSR aerogels prepared at different content of CNT

Samples	Density/ (g·cm⁻³)	Average pore diameter/nm	Specific pore area/(m²·g⁻¹)	T_d10 ^a/℃	T_max ^b/℃	Residues/(900℃,%)
S-0	0.3985	56.02	112.19	486.02	494.07	71.59
SC-2	0.3833	63.50	106.78	525.80	522.86	73.58
SC-5	0.3659	137.39	58.33	545.92	540.13	77.83
SC-10	0.3427	239.70	34.28	558.21	560.28	81.23
SC-15	0.3212	368.20	23.14	597.14	573.24	83.52
Notes：T_d10 is the temperature corresponds to 10% weight loss of the materials; T_max is the temperature corresponds to the maximum pyrolysis rate of the materials.

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表 2 不同QF/SC复合材料的基本性能数据

Table 2. Density and thermal conductivity of QF/SC composites

Samples	Density/ (g·cm⁻³)	Thermal conductivity/ (W/(m·K)⁻¹)
QF/S-0	0.42663	0.054
QF/SC-2	0.42114	0.064
QF/SC-5	0.41384	0.069
QF/SC-10	0.39702	0.075
QF/SC-15	0.37182	0.064

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