Preparation and Properties of High Emissivity Coatings on the Surface of High Thermal Conductivity Cabon/carbon Composites
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摘要: 高导热碳/碳(HTC-C/C)复合材料表面的红外发射率较低，导致其辐射散热能力较差，为进一步提高其热管控能力，需要在其表面涂覆高发射率涂层。通过使用压缩空气喷涂法在HTC-C/C复合材料表面制备了兼具高红外辐射和抗热震性能的碳纳米管(CNTs)/炭黑(CB)复合涂层，在沉积一定量的热解碳(PyC)后，使涂层在保持高红外发射率的同时获得了更强的界面结合性能。探究了热震和高温热处理对高发射率涂层组织和性能的影响。结果表明，当CNTs与CB质量比达到最优比例时，制备得到的涂层发射率达0.94以上，经60次300℃↔−196℃热循环的抗热震性能测试后未发生开裂和剥落现象，具有良好的热稳定性。涂层中的纳米碳材料在热处理后微观有序程度发生改变，导致涂层发射率呈现波长依赖性，但是由于各个波段的协同作用，全测试波段(1-22 μm)发射率波动较小。Abstract: The infrared emissivity of high thermal conductivity carbon/carbon (HTC-C/C) composite surface is low, resulting in poor radiative heat dissipation ability. In order to further improve its thermal control ability, it is necessary to coat its surface with high emissivity coating. Carbon nanotube (CNTs)/carbon black (CB) composite coating with high infrared radiation and thermal shock resistance was prepared on the surface of HTC-C/C composite material by compressed air spraying method. After a certain amount of pyrogenic carbon (PyC) was deposited, the coating obtained stronger interface bonding performance while maintaining high infrared emissivity. The effects of thermal shock and high temperature heat treatment on the microstructure and properties of high emissivity coatings were investigated. The results showed that When the mass ratio of CNTs to CB reached the optimal ratio, the emissivity of the prepared coating reached more than 0.94, and no cracking and spalling occurred after 60 thermal shock resistance tests at 300℃↔−196℃, indicating good thermal stability. After heat treatment, the microstructure order of the nano-carbon materials in the coating changes, resulting in wavelength dependence of the coating emissivity. However, due to the synergistic effect of each band, the emissivity of the whole test band (1-22 μm) fluctuates little.
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图 1 不同原料配比的CNTs/CB复合涂层SEM图及孔隙分布统计图
Figure 1. SEM images of composite coating with different material ratios (a,b,i)CNTS/CB-1;(c,d,j) CNTS/CB-2;(e,f,k)CNTS/CB-3;(g,h,l) CNTS/CB-4
图 2 不同CNTs/CB样品的表面形貌测试
Figure 2. Surface morphology test of different CNTs/CB samples (a)CNTS/CB-1;(b)CNTS/CB-2;(c)CNTS/CB-3;(d)CNTS/CB-4
图 3 不同CNTs/CB样品的红外发射率曲线
Figure 3. Infrared emissivity curves of different CNTs/CB samples
图 4 不同CNTs/CB样品沉积15分钟PyC后的SEM图
Figure 4. SEM images of different CNTs/CB samples after deposited 15 min pyrolytic carbon (a,b)CNTs/CB-PyC-1;(c,d)CNTs/CB-PyC-2;(e,f)CNTs/CB-PyC-3;(g,h)CNTs/CB-PyC-4
图 5 沉积15 min PyC后不同样品的红外发射率曲线
Figure 5. Infrared emissivity curves of different samples after 15 min PyC deposition
图 6 沉积15 min PyC的不同样品经热震实验后的SEM图
Figure 6. SEM images of different PyC samples deposited for 15 min after cycling experiment (a)CNTs/CB-PyC-1;(b) CNTs/CB-PyC-2;(c)CNTs/CB-PyC-3;(d) CNTs/CB-PyC-4
图 7 沉积15 min PyC后各样品划痕测试结合力
Figure 7. After deposition of PyC for 15 min, the binding force of each sample was tested by scratches
图 8 (a) CNTs/CB-PyC复合涂层高温下的红外发射率 (b) CNTs/CB-PyC复合涂层经不同温度热处理后室温下的红外发射率
Figure 8. (a) Infrared emissivity of CNTs/CB-PyC composite coatings at high temperature (b)Infrared emissivity of CNTs/CB-PyC composite coatings at room temperature after heat treatment at different temperatures
图 9 CNTs/CB-PyC-3样品的XRD与拉曼测试结果
Figure 9. XRD and Raman test curves of CNTs/CB-PyC-3 at different heat treatment temperatures (a,c)CB;(b,d)CNTs
图 10 HTC-C/C复合材料喷涂涂层前后的红外热像仪照片
Figure 10. Infrared thermal camera photos before and after HTC-C/C composite coating
表 1 复合涂层的主要组分质量比
Table 1. Mass ratios of main components of composite coatings
Mass Ratio Isopropanol
(IPA)Carbon nanotube
(CNTs)Carbon black (CB) Sodium dodecyl
benzene sulfonate (SDBS)phenolic resin (PF) Samples CNTs/CB-1 1000 4 16 3 2 CNTs/CB-2 1000 8 12 3 2 CNTs/CB-3 1000 12 8 3 2 CNTs/CB-4 1000 16 4 3 2 Notes: The above ratio is the mass ratio of each component in the slurry used for spraying. Only the proportion of CNTs and CB is different, and other conditions are the same. 
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