Flexural strength enhancement study of aluminum-CFRP at liquid nitrogen temperature
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摘要: 随着铝合金-碳纤维增强树脂复合材料(CFRP)逐渐应用到火箭推进器，其低温环境下的粘结性能强化已引起广泛关注。针对环氧接头潜在的粘接界面缺陷，采用阳极氧化和砂化分别处理铝合金和CFRP板表面制得多孔表面。采用树脂预涂(RPC)技术消除铝合金孔道根部原有的大分子环氧树脂空穴缺陷，也可通过RPC技术将增强纤维碳纳米管浸渍到铝合金表面的孔道中，形成准Z方向的纤维桥联，进一步提高环氧接头的粘结强度。三点弯曲试验(3-P-B)结果表明，室温下处理后的铝合金-CFRP弯曲强度提高了14.6%，液氮温度下弯曲强度提高了27.6%。经过表面处理后，CFRP在室温和液氮温度下的破坏模式均由较弱的界面脱胶破坏转变为主体结构的断裂破坏。总之，系列有效的处理方法可为低温液体燃料箱的工业应用提供另一种参考。Abstract: The adhesive bonding strength enhancement of aluminum substrate and carbon fiber reinforced polymer (CFRP) at cryogenic temperature has attracted far-ranging attention with their application expanding to rocket booster. Aiming at the potential bonding interface defect of epoxy joint, we adopted the anodizing and sanding treatments to modify surface performance of Al substrate and CFRP panel respectively. The resin pre-coating (RPC) technique was used to eliminate the originally existing defect caused by macromolecular epoxy at the root of porous Al substrate. The carbon nanotubes were applied as additives to be impregnated into channels on Al substrate surface via RPC technique and construct the quasi-Z directional fiber bridging, which can further improve the adhesive bonding strength of epoxy joint. The three-point bending (3-P-B) results show the flexural strength of aluminum substrate-CFRP after treated has been enhanced by 14.6% at room temperature, and even higher 27.6% at liquid nitrogen temperature based on that of the one only cleaned by acetone. Failure mode exhibits the weaker adhesive failure on bonding interface has been transformed into main structure fracture failure of CFRP after combined surface treatments at both room temperature and liquid nitrogen temperature. Overall, the effective treatment methods can offer an alternative reference in industrial application of cryogenic liquid fuel tank.
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图 1 经阳极氧化、磨砂和树脂预涂(RPC)处理后的Al-CFRP复合材料优化设计方案
Figure 1. Optimized design schematic of Al substrate-CFRP composite after treated via anodizing, sanding and resin pre-coating (RPC)
CFRP—Carbon fiber reinforced polymer; CNTs—Carbon nanotubes
图 2 铝合金阳极氧化处理工艺与相关化学反应
Figure 2. Treatment process and relevant chemical reactions of anodizing treatment on Al substrate
图 3 室温和液氮温度下的三点弯曲(3-P-B)试验模型
Figure 3. Three-point bending (3-P-B) test models at room temperature and liquid nitrogen temperature
图 4 6060 T5铝合金的SEM图像：(a) 铝合金表面丙酮超声清洗；(b) 阳极氧化后的铝合金表面具有较深的微/纳米结构通道；(c) 阳极氧化后的铝合金52°视角图像；(d) 聚焦离子束(FIB)处理后多孔铝合金表面切口壁的正面图；(e)、(f) RPC处理后CNTs嵌入到铝合金表面孔道结构[32]
Figure 4. SEM images of 6060 T5 Al substrate: (a) Al substrate surface with acetone ultrasonic cleaning; (b) Al substrate surface with deep micro-/nano-structured channels after anodizing treatment; (c) 52° view image of the Al substrate after anodized corresponding to (b); (d) Frontal view of the notched wall on porous Al substrate surface after focus ion beam (FIB); (e),(f) CNTs inserted into the channel of Al substrate surface after RPC technique[32]
图 5 铝合金的AFM图像：(a)、(b)经丙酮超声清洗的试样的两个不同位置；(c)、(d)经阳极氧化处理的试样的两个不同位置
Figure 5. AFM images of Al substrates: (a), (b) Two different positions of the same sample cleaned ultrasonically by acetone; (c), (d) Same sample after anodizing treatment
图 6 丙酮超声清洗和阳极氧化的铝合金表面的光谱分析 (a) ；丙酮超声清洗 (b) 和阳极氧化处理后铝合金表面 (c) 的高分辨Al2p核心级光谱
Figure 6. Survey spectra of Al substrate surfaces cleaned ultrasonically by acetone and anodized (a); high resolution Al2p core-level spectra for Al substrate surfaces after acetone ultrasonic cleaning (b) andanodizing treatment (c)
Aloh—Aluminium hydroxide hydroxide; Almet—Metallic aluminium; Alox—Aluminium oxide
图 7 在室温和液氮温度下完成3-P-B试验后的对照组和增强效果最优的实验组Al-CFRP复合材料：(a) 典型的力与位移曲线；(b) 弯曲强度
Figure 7. Control and optimal Al-CFRP composites after 3-P-B tests at both room temperature and liquid nitrogen temperature: (a) Typical load-displacement curves; (b) Flexural strength values
图 8 Al-CFRP复合材料三点弯曲试验后的部分粘合及分离的失效表面：(a) 丙酮超声清洗后的铝合金和CFRP板；(b) 铝合金经过阳极氧化和RPC(添加碳纳米管)，CFRP板经过砂纸打磨和RPC
Figure 8. Failure surfaces of adhesive bonded Al-CFRP composite and the separated pieces: (a) Acetone ultrasonic cleaning for Al substrate and CFRP; (b) Anodized Al substrate with RPC + CNTs and sanding and RPC for CFRP
图 9 Al-CFRP复合材料的粘接表面失效模式示意图：(a) 仅经过丙酮超声清洗的铝合金与CFRP板呈现出典型的脱胶失效；(b) 经过阳极氧化和RPC(添加碳纳米管)的铝合金与经过砂纸打磨和RPC的CFRP板呈现出碳纤维基体的断裂失效
Figure 9. Schematic diagram of failure mode on Al substrate and CFRP adhesive surface: (a) Typical adhesive failure only with acetone ultrasonic cleaning for Al substrate and CFRP; (b) CFRP fracture failure with anodizing + RPC with carbon nanotubes for Al substrate and sanding + RPC for CFRP
CFRP—Carbon fiber reinforced polymer; CNTs—Carbon nanotubes
表 1 经丙酮超声清洗和阳极氧化处理后6060 T5铝合金的表面粗糙度参数
Table 1. Surface roughness measurements of the 6060 T5 Al substrate treated by acetone ultrasonic cleaning and anodizing
Treatment method Sample number Sa/nm Sq/nm Rmax/nm Acetone ultrasonic cleaning Fig.5(a) 53.4 62.5 353 Fig.5(b) 36.5 42.9 238 Anodizing surface treatment Fig.5(c) 91.3 114 785 Fig.5(d) 95.4 134 1037 Notes: Sa—Surface arithmetical mean roughness; Sq—Surface root mean square roughness; Rmax—Maximum roughness depth. 
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表 2 丙酮清洗和阳极氧化后铝合金上超薄表面层的表面元素组成
Table 2. Surface elemental composition of the ultra-thin surface layer on both acetone-cleaned and anodized Al substrates
Sample Almet Alox Aloh Acetone-cleaned Al substrate 21.0% 62.7% 17.5% Anodized Al substrate − − 100.0%
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表 3 室温(RT)和液氮温度(LNT)下对照组和实验组Al-CFRP复合材料的3-P-B试验结果
Table 3. 3-P-B test results of control and treated Al-CFRP composites at room temperature (RT) and liquid nitrogen temperature (LNT)
Sample Treatment process Test
conditionAverage
Pmax/NStandard
deviation/NShear
strength/MPaStandard
deviation/MPaControl Acetone ultrasonic cleaning for both RT 2564.21 136.87 269.97 48.14 LNT 2915.79 591.69 532.92 60.51 T1 Anodizing for Al and Acetone ultrasonic cleaning for CFRP RT 2690.45 142.53 285.76 23.42 LNT 5364.05 514.17 569.73 49.64 T2 Anodizing for Al and sanding +
RPC for CFRPRT 2760.61 121.31 290.15 17.75 LNT 5541.01 531.58 582.38 42.73 T3 Anodizing for Al and RPC (CNTs) sanding + RPC for CFRP RT 5015.57 109.55 309.31 13.05 LNT 6374.42 545.44 680.01 48.14 Note: Pmax—Maximum peak load.
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