Research progress and perspective on bonding technologies of metal/CFRP materials and its interfacial bonding mechanism
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摘要: 碳纤维复合材料(CFRP)具有质轻高强、高模量和低膨胀优势，在“陆海空天”等领域应用潜力和需求极大. 其中热塑性碳纤维复合材料(CFRTP)近年来快速发展，CFRP和CFRTP与金属结构件的连接技术受到国内外学者和工业界的广泛关注. 文中综述了金属材料与CFRP连接的主要技术及界面的结合机理；对比分析了不同连接工艺的成形原理，总结了金属与CFRP连接界面的不同作用效果；结合发展现状及未来工程应用需求，对金属/CFRP高质量连接技术瓶颈的突破方向进行了展望.
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关键词:
- 金属/碳纤维复合材料 /
- 黏接 /
- 机械紧固 /
- 异种材料连接 /
- 界面结合机理
Abstract: Carbon fiber reinforced polymer (CFRP) has been applied in the fields of land, sea, air, and space due to advantages of light weight, high modulus, and low expansion. In recent years, with the development of carbon fiber reinforced thermoplastic plastics (CFRTP), bonding technologies for CFRPs and metals have gained extensive attention from domestic and foreign industry and scholars. This study summarizes the main technologies and bonding mechanisms of metal/CFRP. In addition, the forming principles of different bonding processes were analyzed, and contributing factors at the interface between metals and CFRPs were summarized. Furthermore, the technical breakthrough direction of high-quality metal/CFRP connections was explored based on development status and engineering application needs. -
0. 序言
核反应堆包层结构经受着极其恶劣的服役环境，要求其在长期服役过程中保持结构和冶金的完整性. 9Cr-1.5W-0.15Ta耐热钢具有较低的辐照肿胀系数和热膨胀系数、较高的热导率等优异的热物理性能和良好的力学性能，被认为是核聚变/裂变发堆包层结构的理想候选材料之一[1-4].
为了减小热影响区宽度，保持接头良好的组织性能，多采用低热输入、高能量密度的特种焊接技术对9Cr-1.5W-0.15Ta耐热钢进行焊接[5-7]. 搅拌摩擦焊(Friction stir welding, FSW)是一种新型固态塑性连接技术，焊接热输入较低，可以保持焊缝性能与母材相近，焊接变形和残余应力较小等的特点[8-9]. 与搅拌摩擦焊相比，电子束焊(electron beam welding，EBW)是一种高效率、高能量密度的熔化焊接方法，具有焊接冶金质量好、焊接熔深大和焊接热影响区窄的特点，具有适用性强、操作简便等优势[10-11]. 因此，对比研究9Cr-1.5W-0.15Ta耐热钢搅拌摩擦焊缝和电子束焊缝组织和力学性能的差异具有重要意义.
文中对9Cr-1.5W-0.15Ta耐热钢电子束焊缝和搅拌摩擦焊缝的微观组织、硬度和冲击性能进行比较，分析微观组织与力学性能之间的关联性，并论述接头的断裂机制.
1. 试验方法
试验采用的母材为9Cr-1.5W-0.15Ta耐热钢，其化学成分如表1所示. 母材热处理工艺如下：1000 ℃下正火保温60 min，水淬之后在700 ℃下回火60 min. 搅拌摩擦焊机为北京赛福斯特技术有限公司生产的FSW-3LM-020型设备，搅拌头的材料为W-25%Re合金. 焊接工艺参数为焊接速度60 mm/min，焊接转速300 r/min和焊接压力10 kN. 电子束焊机选择KL110型真空电子束焊机设备. 焊接加速电压60 kV，焊接电流30 mA，焊接速度600 mm/min，在全聚焦状态下以束流垂直于板面的方式进行焊接.
沿垂直于焊接方向切取尺寸为25 mm × 10 mm的试样，经过粗磨、细磨和抛光后，在5 g FeCl3, 20 mL盐酸和100 mL蒸馏水的腐蚀液中侵蚀90 s制备金相试样. 采用光学显微镜(OLYMPUS GX51)和电子扫描显微镜(SEM，TDCLSU 1510)对接头区域的微观组织进行观察. 采用型号为Tecnai G2F30透射电子显微镜在300 kV加速电压下观测析出相.
低温冲击试验试样尺寸如图1所示，冲击试验后，采用电子扫描显微镜观测冲击试样断口形貌. 硬度试验是在金相试样上焊缝区域测试，载荷为9.8 N，加载时间为15 s.
表 1 9Cr-1.5W-0.15Ta耐热钢化学成分(质量分数，%)Table 1. Chemical composition of the 9Cr-1.5W-0.15Ta heat resistant steelC Cr Mn V W Ta Si Zr N S P Fe 0.1 9 0.5 0.2 1.5 0.15 0.05 0.005 0.007 0.002 0.002 余量 ![]()
图 1 焊缝低温冲击试样取样位置和几何尺寸(mm)Figure 1. Dimension and position of impact toughness testing sample in the weld2. 试验结果与分析
2.1 微观组织
9Cr-1.5W-0.15Ta耐热钢母材、电子束焊缝和搅拌摩擦焊缝的微观组织如图2所示. 图2a, b是9Cr-1.5W-0.15Ta耐热钢母材的微观组织，由于经过正火、淬火和回火等热处理后，具有完全的回火的组织特征，晶粒尺寸大约为20 μm，并在原奥氏体晶界和晶内形成均匀分布的析出相(M23C6和MX). 电子束焊缝的微观组织如图2c, d所示，其特点为晶粒粗大，组织不均匀，且晶界处的M23C6析出相和晶内MX析出相均发生完全溶解. 虽然电子束焊能量密度较大，熔池中心温度高，但其高温停留时间短，焊后冷却速度较大，因此在熔合线形成较大的温度梯度，促进粗大的树枝状组织的形成. 从焊缝两边生长的晶粒在焊缝中心处相遇，形成了垂直于母材原始晶粒取向的组织结构.
图2e, f为搅拌摩擦焊缝的微观组织. 在焊接过程中，焊缝由于受到搅拌针剧烈的搅拌而引起严重的塑性变形和摩擦，产生的局部高温作用使得组织发生动态再结晶，加之焊后冷却速率较大，发生马氏体转变[12]. 因此，搅拌摩擦焊缝的组织由回火组织转变为板条马氏体. 焊缝区域晶粒发生明显细化，这是由于该区域受到搅拌针的机械作用，动态再结晶的晶粒发生破碎而细化. 此外，在搅拌摩擦焊缝中晶界上的M23C6析出相发生完全溶解，而晶内依然存在球状MX析出相，这表明焊缝区域经历的焊接热循环峰值温度高于M23C6相的熔点(860 ℃)、但低于MX相熔点(1310 ℃)[13-14].
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图 2 母材、电子束焊缝和搅拌摩擦焊缝的微观组织特征Figure 2. Microstructure of base metal, EBW weld and FSW weld. (a) metallographic of base metal; (b) SEM microstructure of base metal; (c) metallographic of EBW weld; (d) SEM microstructure of EBW weld; (e) metallographic of FSW weld; (f) SEM microstructure of FSW weld图3为母材和搅拌摩擦焊缝中析出相特征. 母材中M23C6碳化物和球状MX相分别均匀地分布在原奥氏体晶界和晶内(图3a, b). 焊后晶界处M23C6碳化物发生完全溶解，球状MX碳氮化物无明显变化，但对位错产生强烈的钉扎作用，同时在板条马氏体内生成大量的针状M3C相，主要由W，Cr，Fe和C组成(图3c ~ 3f). 这主要是由于M23C6碳化物的溶解在晶界和晶内之间产生C和Cr原子的浓度梯度，同时焊接过程中的奥氏体化再结晶和马氏体转变诱导位错和空位等晶格缺陷增殖，为针状M3C碳化物析出提供了形核质点和原子扩散通道，促进了M3C碳化物的析出[15].
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图 3 母材和搅拌摩擦焊缝析出相的特征Figure 3. Characteristics of precipitates for base metal and FSW weld. (a) M23C6 phase in base metal; (b) MX phase in base metal; (c) M23C6 phase in FSW weld; (d) MX phase in FSW weld; (e) M3C phase in FSW weld; (f) energy spectrum of M3C phase2.2 力学性能
2.2.1 显微硬度
表2为母材、电子束焊缝和搅拌摩擦焊缝硬度结果. 相比于9Cr-1.5W-0.15Ta耐热钢的硬度(272 HV)，两种焊缝的硬度明显增大，电子束焊缝硬度值为475 HV，搅拌摩擦焊缝硬度值为425 HV. 焊缝区明显硬化，这是由于在焊接过程中焊接热循环峰值温度高于母材的相变温度，在焊后快速冷却导致焊缝中形成大量的板条状马氏体组织，使得焊缝的硬度增大[16-17].
表 2 母材、电子束焊缝和搅拌摩擦焊缝显微硬度(HV)Table 2. Microhardness of the base metal, EB and FSW welds母材 EBW焊缝 FSW焊缝 272 475 425 2.2.2 冲击韧性
图4是9Cr-1.5W-0.15Ta耐热钢母材、电子束焊缝和搅拌摩擦焊缝在−20 ℃下的冲击吸收能量. 由图可知，母材的冲击吸收能量为34.35 J，搅拌摩擦焊焊缝冲击吸收能量为31.1 J，而电子束焊焊缝的冲击吸收能量为4.2 J，仅为母材的12.2%和搅拌摩擦焊缝的13.5%.
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图 4 母材、电子束焊缝和搅拌摩擦焊缝在−20 ℃下的冲击韧性Figure 4. Impact toughness of base materials, EBW and FSW welds at −20 ℃接头的力学性能主要取决于其微观组织特征. 与母材相比，搅拌摩擦焊接头韧性稍有降低，这是焊缝区晶粒细化、高角度晶界增加阻碍裂纹扩展而改善接头韧性和位错密度增加而恶化冲击性能的共同结果[18-20]. 除此之外，残余奥氏体的存在也对改善接头韧性具有重要影响[21]. 相比于搅拌摩擦焊接头，电子束焊接头韧性显著降低，这主要是由于在焊缝中树枝状组织的形成，使焊缝韧性明显降低. 另外，电子束焊接过程中热输入较大，引起晶粒粗化和析出相溶解等组织变化，对接头的冲击韧性产生重要影响.
2.2.3 冲击断口形貌
图5为母材、电子束焊缝和搅拌摩擦焊缝试样冲击后的断口形貌. 由于微观组织特征的差异，导致焊接接头力学性能的不同，同时也在冲击断口形貌上表现明显的不同. 母材的冲击断口形貌表现为典型的韧窝特征，并且韧窝大小和形状存在明显差别，发现小尺寸韧窝密度远多于大尺寸韧窝(图5a). 电子束焊缝冲击断口则表现为典型的解理断裂，同时局部还可以发现较深的裂纹(图5b). 搅拌摩擦焊缝冲击断口形貌均表现为大小和形状均匀的韧窝特征，在部分韧窝底部存在第二相粒子脱落的现象，并且由于冲击变形而形成少量的撕裂痕，断裂方式属于微孔聚集型断裂(图5c). 综上，母材和搅拌摩擦焊缝的冲击断裂方式属于典型的延性断裂，而电子束焊缝的冲击断裂方式属于脆性断裂.
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图 5 冲击试样的断口形貌Figure 5. Fracture morphology of impact specimens. (a) base metal; (b) EBW weld; (c) FSW weld电子束焊缝和搅拌摩擦焊缝的冲击断口形貌与母材有不同程度的差异. 在搅拌摩擦焊缝中，由于发生动态再结晶，晶粒尺寸明显细化，同时仅部分低熔点析出相溶解，冲击断口表现尺寸较大的韧窝特征，导致冲击韧性发生稍稍降低. 然而，对于电子束焊缝，微观组织为粗大的树枝状晶，并且析出相均发生溶解，导致在冲击过程中协调变形能力变弱，断口表现为典型的解理断裂特征. 因此，电子束焊缝的冲击韧性显著降低.
3. 结论
(1) 9Cr-1.5W-0.15Ta耐热钢电子束焊缝呈树枝状晶微观组织，晶粒粗大，组织不均匀，且析出相均发生溶解；搅拌摩擦焊缝则由细小、均匀的板条马氏体微观组织组成，部分晶界析出相发生溶解.
(2) 由于在焊缝中有大量板条马氏体生成，9Cr-1.5W-0.15Ta耐热钢电子束焊缝和搅拌摩擦焊缝的硬度值均发生了显著增大，电子束焊缝的硬度值最高可达到475 HV.
(3) 两种焊缝的冲击韧性均低于母材，但由于电子束焊缝和搅拌摩擦焊缝中晶粒尺寸、析出相的差异，不同焊缝表现不同的力学性能. 电子束焊缝的冲击吸收能量仅为母材的12.2%；搅拌摩擦焊缝的力学性能较好，其冲击吸收能量为母材的90%.
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图 3 金属/CFRP螺栓连接技术和铆钉连接技术
Figure 3. Metal/CFRP bolting technology and riveting technology
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图 4 金属/CFRP搅拌摩擦盲铆连接技术[29]
Figure 4. Metal/CFRP friction stir blind riveting technology
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图 6 金属/CFRP制备技术中的机械锁合效果
Figure 6. The mechanical locking of metal/CFRP. (a) vertical blind riveting; (b) self-punch riveting; (c) hot riveting
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图 7 金属/CFRTP单侧电阻点焊连接技术
Figure 7. Metal/CFRTP one-sided resistance spot welding technology
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图 9 金属/CFRTP异质界面的化学键合以及冶金结合原理
Figure 9. Chemical bonding and metallurgical bonding principles at the metal/CFRTP heterogeneous interface
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图 10 采用不同连接技术CFRP/金属连接界面的结合强度分布
Figure 10. The bonding strength distribution of CFRP/metal connection interface of different bonding technologies
表 1 不同黏接剂连接金属/CFRP复合材料性能
Table 1 Properties of different adhesives bonding of metal/CFRP composite materials
黏接剂名称 黏接剂类型 金属材质 CFRP材质 最优黏接强度τ /MPa TGJ[7] 环氧树脂 Q235钢 UT70-30 3.36 DP 490[8] 环氧树脂 7075铝合金 CFRP — Sikadur 330[9] 双组份环氧树脂 Q235钢 EP/CF 10.4 J-241[11] 改性环氧树脂 铝合金 EP/CF 16.5 J133[12] 改性环氧树脂 钛合金 CFRP 19.83 SY-300K[13] 改性环氧树脂 铝合金 BMI/CF 21.9 EA E-20HP[18] 双组份环氧树脂 A6061-T6铝合金 CFRP 16 Araldite 420[20] 环氧树脂 低碳钢 CFRP 35 DP 460[21] 增韧环氧树脂 7075铝合金 3K-T700 11.49 DP 460[22] 增韧环氧树脂 7075铝合金 EP/CF 23.63 
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表 2 CFRP与金属连接材料的组合类别
Table 2 The combining forms of CFRP/metal bonding
连接方式 钛合金 铌合金 镁合金 铝合金 钢 不锈钢 黏接 参考文献[12, 16] — — 参考文献[8, 11, 13-15, 17-19, 21-22] 参考文献[7, 9, 10, 20] — 螺栓连接 — — — 参考文献[23-24] — — 铆接 参考文献[26, 30-31] — 参考文献[32] 参考文献[28-29] 参考文献[25] — 钎焊 参考文献[38-39] 参考文献[38] — 参考文献[35-37] — — 电阻焊 — — — 参考文献[40, 42] — 参考文献[41] 超声波焊 — — 参考文献[45] 参考文献[43, 44, 46] — — 激光焊 参考文献[49, 50, 56] — — 参考文献[48, 51-52] 参考文献[55] 参考文献[53-54] 搅拌摩擦焊 — — 参考文献[62] 参考文献[57-61, 63-64, 68] 参考文献[69] —
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