Vacuum brazing TC4 titanium alloy / 316L stainless steel with Ti43.76Zr12.50Cu37.49-xNi6.25Cox amorphous filler metals
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摘要:
根据双团簇模型设计并制备了Ti-Zr-Cu-Ni-Co系非晶钎料，用于真空钎焊TC4钛合金和316L不锈钢，分析了钎料中Co元素含量对钎焊接头界面微观组织形貌、力学性能及断裂行为的影响规律.结果表明，钎焊接头可划分为TC4/扩散区(I区)/钎缝中心区(II区)/界面区(III区)/316L，界面典型微观组织结构为TC4/β-Ti + Ti2Cu/(Ti, Zr)2(Cu, Ni) + Ti2Cu + Ti2(Cu, Ni) + TiFe/(Fe, Cr)2Ti + α-(Fe, Cr) + τ + γ-(Fe, Ni) + σ/316L，随着Co元素含量的增加，接头剪切强度先升高后降低再升高，当Co元素含量为1.56%时达到最大310 MPa，不添加Co元素时，接头断裂于钎缝中心区(II区)；当Co元素含量为1.56% ~ 6.24%时，接头断裂于靠近316L母材的界面区(III区)附近，断裂模式为典型的解理断裂.
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关键词:
- 真空钎焊 /
- 非晶钎料 /
- 钛合金/不锈钢异种金属 /
- 微观组织 /
- 剪切强度
Abstract:Ti-Zr-Cu-Ni-Co amorphous filler metals were designed and prepared for vacuum brazing of TC4 titanium alloy to 316L stainless steel according to the dual-cluster model. The effect of Co content in filler metals on the microstructure, mechanical properties and fracture behavior of brazed joints was investigated. The results showed that the cross section of brazed joint could be divided into TC4/diffusion zone I/brazing seam center zone II/interface zone III/316L. The typical interfacial microstructure of the brazed joints was TC4/β-Ti + Ti2Cu/(Ti, Zr)2(Cu, Ni) + Ti2Cu + Ti2(Cu, Ni) + TiFe/(Fe, Cr)2Ti + α-(Fe, Cr) + τ + γ -(Fe, Ni) + σ/316L. The shear strength of brazed joints first increased, then decreased and then increased with the increase of Co content. The maximum shear strength of 310 MPa was obtained at 1.56% Co. When Co element was not added, brazed joints fractured in the center of the brazing seam (zone II). And when the Co content was 1.56 ~ 6.24%, brazed joints fractured near the interface zone (zone III) of 316L base metal. The fracture mode was typical cleavage fracture.
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0. 序言
随着电子元器件封装密度的增加，陶瓷球栅阵列(CBGA)和陶瓷柱栅阵列(CCGA)因其高密度的面排布引脚形式，在航空航天等高可靠性领域产品中得到了广泛应用[1-2]. CBGA和CCGA封装器件分别通过陶瓷管壳上的焊球和焊柱实现与PCB基板的组装互连，由于氧化铝陶瓷管壳(热膨胀系数为6.5 × 10−6/℃)和PCB基板(热膨胀系数为18 × 10−6 ~ 21 × 10−6/℃)的热膨胀系数差了近3倍，这种差异会在温度变化过程中产生剪切应变而导致裂纹萌生，进而引发焊点失效，因此温度循环成为了封装器件可靠性评估的关键手段. CCGA封装是在CBGA封装的基础上，用柱栅阵列代替了球栅阵列，增加互连引脚的距离，大大缓解了热膨胀系数不匹配带来的焊点失效问题，提高了焊点的可靠性，成为大尺寸产品封装的更优选择[3-5].
在温度循环过程中，焊点的界面显微组织会发生变化，包括金属间化合物(IMC)的成分及厚度等[6-8]，界面的显微组织会影响焊点的可靠性，焊点的抗剪强度是反映其可靠性最直观的方式，因此分析温度循环过程中焊点的显微组织与抗剪强度的演变关系对揭示CCGA封装焊点的失效机理及建立可靠性评估依据具有重要的参考价值.
文中以CCGA484封装器件为研究对象，分析温度循环过程中焊点的界面显微组织演变与抗剪强度的对应关系，研究温度循环过程中焊点的失效机理，为CCGA封装的发展及应用提供理论指导.
1. 试验方法
1.1 原材料及试验样品制备
试验中选用高温共烧氧化铝陶瓷外壳，型号为CLGA484，镀层为Ni/Au，焊盘直径为ϕ0.8 mm ± 0.05 mm，焊盘间距为1.27 mm，板级封装用PCB板上的焊盘直径为ϕ0.8 mm ± 0.05 mm，焊柱采用ϕ0.51 mm × 2.21 mm的Pb90Sn10普通高铅焊柱，植柱和组装到PCB板上采用的锡膏均采用Sn63Pb37.
试验样品制备过程为：丝网印刷锡膏→植柱→真空回流焊接→清洗→PCB板喷印锡膏→CCGA器件与PCB焊盘喷印锡膏光学对位→真空回流焊接，完成板级封装后的试验样品如图1所示，将组装到PCB板的试样与未组装的CCGA器件同时进行温度循环试验，前者用于观察不同温度循环次数下焊柱的外观形貌，后者用于焊点的金相分析和剪切力测试.
1.2 温度循环条件
对CCGA484试验样品进行温度循环试验，试验条件按照美军标MIL-STD-883. 温度循环曲线如图2所示，温度范围为−65 ~ 150 ℃，循环周期为50 min，高低温保温时间均为15 min，升降温速率相同，试验过程中，每隔100次温度循环取出进行形貌观察、剪切力测试和金相分析，共进行500次温度循环.
1.3 抗剪强度测试
选用抗剪强度作为CCGA焊点的可靠性评估依据，试验设备采用专门的微焊点强度测试仪(DAGE4800)，剪切速度均为0.4 mm/s，由于CCGA484器件的焊柱间距较小，试验过程中需要铲去周围的焊柱，保证剪切工具在行进时不会接触其它材料.
2. 试验结果与分析
2.1 焊柱宏观形貌演变分析
由于陶瓷管壳和PCB板的热膨胀系数差别较大，这种热失配会在温度变化过程中产生剪切应变，宏观表现为焊柱发生塑性变形.
温度循环过程中焊柱形貌如图3所示. 从图中可以看出，温度循环次数达到400次时，焊柱在反复热冲击作用下开始发生明显的塑性变形，且表面变得更加粗糙，焊点位置伴随有轻微的颈缩现象，500次后焊柱的扭曲程度进一步加剧，但肉眼还未观察到焊点开裂现象.
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图 3 不同温度循环次数下CCGA封装器件的宏观形貌Figure 3. Evolution of solder column morphology at different thermal cycling times. (a) 100 times; (b) 300 times; (c) 400 times; (d) 500 times由于焊柱在长时间的高温、恒压力作用下，即使应力小于屈服强度也会慢慢发生蠕变变形[9]. 在温度循环的升温及高温保温阶段，陶瓷的热膨胀系数大于PCB基板，焊柱发生倾斜，在温度循环的降温及低温保温阶段，焊柱恢复至初始状态后向相反方向偏移，在反复的升温降温过程中，焊柱蠕变变形逐渐累积，达到宏观可见的扭曲状态，而焊点钎料的强度要略大于焊柱，因此在焊点处会有颈缩现象产生.
2.2 焊点显微组织分析
在焊点形成过程中，钎料与焊盘金属在短时间的高温作用下扩散生成硬脆的IMC层，实现焊柱与基板之间的电气和机械连接，但是在长时间的温度循环过程中，扩散作用导致IMC层厚度逐渐增加，其成分也会发生相应的变化，由于IMC的热膨胀系数与钎料相差较大，因此过厚的IMC会对焊点的可靠性产生不利的影响.
不同温度循环次数下的CCGA焊点界面显微组织如图4所示，在温度循环前，高铅焊柱与Ni焊盘界面观察不到明显的IMC层，因为Ni相对稳定，其界面反应层与铜相比是相当薄的，所以观察不到，随着循环次数增加，界面出现不同颜色对比度的中间层，且厚度逐渐增加，根据Ni-Sn二元相图可知，Sn-Pb钎料与Ni焊盘扩散反应生成的界面IMC从Ni侧依次包括Ni3Sn，Ni3Sn2和Ni3Sn4，具体的化合物成分取决于Sn与Ni的相对浓度.
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图 4 CCGA封装器件焊点显微组织Figure 4. Microstructure of CCGA solder joints at different thermal cycling times. (a) original; (b) 100 times; (c) 200 times; (d) 300 times采用EDS分析界面IMC成分，不同温度循环次数下测试IMC成分的位置如图5 ~ 图7所示，对应不同位置的成分如表1所示. 从图中可以看出，100次温度循环时，界面点1主要为偏析的富锡相，点2处Ni与Sn的原子比接近3∶4，结合Ni-Sn二元相图可知，应为Ni3Sn4化合物，与已有的研究一致[8]；在200次温度循环后，界面点1处仍为Ni3Sn4相，靠近Ni焊盘侧的点2处Ni与Sn的原子比接近3∶2，推测为Ni3Sn2相；500次温度循环后，在Ni与Ni3Sn2相之间的点2处，Ni与Sn的原子比接近3∶1，应为Ni3Sn相，因此推测随着温度循环次数增加，从焊柱到Ni焊盘之间依次生成的IMC为富锡相→Ni3Sn4→Ni3Sn2→Ni3Sn. 分析IMC形成过程，认为在温度循环前，富锡相与Ni通过元素相互扩散，反应生成极少量Ni3Sn4化合物层，Ni3Sn4化合物层的生成阻挡了Sn与Ni的扩散反应，Ni与Ni3Sn4化合物层中微量的Sn继续发生扩散反应，生成Ni含量更高的Ni3Sn2化合物相，之后，Ni3Sn2化合物层进一步阻挡Ni3Sn4化合物层中Sn与Ni的扩散反应，生成Ni含量更高的Ni3Sn化合物相. 统计不同温度循环次数下界面IMC厚度，如图8所示，两者基本呈指数为1/2的幂函数增长关系，符合扩散控制机制.
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图 5 温度循环100次焊点界面IMC成分Figure 5. IMC component of CCGA solder joints at thermal cycling of 100 times![]()
图 7 温度循环500次焊点界面IMC成分Figure 7. IMC component of CCGA solder joints at thermal cycling of 500 times![]()
图 6 温度循环200次焊点界面IMC成分Figure 6. IMC component of CCGA solder joints at thermal cycling of 200 times界面IMC层存在离子键或共价键，所以往往具有硬脆特性，与基板和焊柱的线膨胀系数差别较大，随着温度循环次数增加，硬脆的IMC层厚度会逐渐增加，因此焊点界面处会产生较大的应力集中，在反复热应力作用下会萌生不同方向的细微裂纹，如图7所示，推测随着温度循环次数继续增加，应力集中导致微裂纹沿着剪切应变方向逐渐扩展，直到覆盖整个焊点，导致基板与焊柱之间发生断裂失效.
表 1 不同温度循环次数下焊点界面的成分分析Table 1. Component of CCGA solder joints at different thermal cycling times循环次数 界面点 质量分数w(%) 原子分数a(%) Pb Sn Ni Pb Sn Ni 100 点1 13.43 76.39 10.18 7.35 72.99 19.66 点2 4.97 69.37 25.66 2.3 55.9 41.8 200 点1 9 64.83 26.17 4.2 52.75 43.05 点2 4.91 51.99 43.1 1.93 35.63 62.44 500 点1 8.77 45.44 45.79 3.51 31.77 64.72 点2 8.24 28.16 63.6 2.92 17.44 79.64 ![]()
图 8 温度循环次数与界面IMC厚度的关系Figure 8. Variations of IMC thickness of CCGA solder joint with different thermal cycling times2.3 抗剪强度测试结果与分析
焊点的力学性能是评估其可靠性的最直观方法之一，采用DAGE4800微焊点强度测试仪测试不同循环次数下焊点的抗剪强度，如图9所示. 随着温度循环次数的增加，CCGA封装焊点的抗剪强度呈现下降趋势，到500次温度循环结束，抗剪强度相对下降了15.6%，且下降的速率逐渐增大. 结合上文界面显微组织分析可知，长时间高温会促进界面元素相互扩散，依次生成Ni3Sn4，Ni3Sn2和Ni3Sn多种IMC化合物层，且IMC层厚度逐渐增加，这些化合物与Sn，Pb的晶格常数和晶格结构存在较大差异，具有较高的熔点，呈现硬脆特性，因此在反复塑性变形过程中会产生应力集中，容易萌生裂纹而导致焊点失效，所以焊点的力学性能随着IMC厚度增加而逐渐下降，与已有的研究结果一致[10]. 对抗剪强度Rτ与温度循环次数n之间的关系做曲线拟合，得到下式，即
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图 9 不同循环次数下焊点剪切力变化Figure 9. Variations of shear strength of CCGA solder joints with different thermal cycling times$${R_\tau } = 682.25 - 0.06\;n - 2.77 \times {10^{ - 4}}{n^2}$$ (1) 根据技术指标要求，焊柱的最小剪切力为5.6 N，由式(1)推算可得，当温度循环次数大于550次时，焊点的抗剪强度将不满足要求.
3. 结论
(1) 温度循环超过400次时，CCGA器件焊柱开始发生明显的塑性变形.
(2) CCGA封装器件的焊点随着温度循环次数增加，从Ni焊盘侧依次生成的IMC层成分为Ni3Sn→Ni3Sn2→Ni3Sn4，且IMC层厚度逐渐增加.
(3) CCGA封装器件焊点的抗剪强度随着温度循环次数增加呈下降趋势，且下降的速率逐渐增大，到500次温度循环结束，抗剪强度相对下降了15.6%，这是由于硬脆的IMC层厚度增加，在变形过程中导致应力集中而引发焊点失效.
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图 1 母材的微观组织和XRD图谱
Figure 1. Microstructure and XRD patterns of base metals. (a) TC4 microstructure; (b) 316L microstructure; (c) TC4 XRD; (d) 316L XRD
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图 2 Ti-Zr-Cu-Ni-Co系非晶钎料
Figure 2. Ti-Zr-Cu-Ni-Co Ingots amorphous filler metals. (a) ingots; (b) width; (c) thickness
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图 3 钎焊装配和剪切夹具示意图
Figure 3. Schematic diagram of brazing assembly and shear test fixture. (a) brazing assembly; (b) shear test fixture
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图 5 Ti-Zr-Cu-Ni-Co系非晶钎料表征
Figure 5. Ti-Zr-Cu-Ni-Co amorphous filler metals. (a) XRD patterns; (b) DTA curves
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图 6 Ti43.76Zr12.50Cu35.93Ni6.25Co1.56钎料钎焊接头的微观组织
Figure 6. Microstructure of brazed joint with Ti43.76Zr12.50Cu35.93Ni6.25Co1.56 filler metal. (a) low-magnification image of the joint and (b) magnified image of zone b in a
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图 7 采用Ti43.76Zr12.50Cu35.93Ni6.25Co1.56非晶钎料钎焊接头的元素分布
Figure 7. Elemental distribution of brazed joint with Ti43.76Zr12.50Cu35.93Ni6.25Co1.56 amorphous filler metal
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图 8 采用Ti43.76Zr12.50Cu35.93Ni6.25Co1.56非晶钎料钎焊接头316L母材侧的元素分布
Figure 8. Elemental distribution at 316L base metal side of brazed joint with Ti43.76Zr12.50Cu35.93Ni6.25Co1.56 amorphous filler metal
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图 9 采用Ti43.76Zr12.50Cu35.93Ni6.25Co1.56非晶钎料钎焊接头元素线扫描分布
Figure 9. Elemental line scanning distribution of brazed joint with Ti43.76Zr12.50Cu35.93Ni6.25Co1.56 amorphous filler metal. (a) integral joint; (b) magnified image of zone b in 9(a)
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图 10 950 ℃/10 min条件下不同Co含量非晶钎料钎焊接头界面微观组织
Figure 10. Effect of Co content in filler metals on interfacial microstructure of brazed joint at 950 ℃/10 min. (a) 0%; (b) 1.56%; (c) 3.12%; (d) 4.68%; (e) 6.24%
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图 11 不同Co元素含量钎焊接头III区Ti-Fe化合物层的厚度
Figure 11. Thickness of Ti-Fe reaction layer in zone III of brazed joints with different Co content
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图 12 950 ℃/10 min条件下不同Co元素含量非晶钎料钎焊接头的剪切强度
Figure 12. Shear strength of brazed joints with different Co content filler metals at 950 ℃/10 min
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图 13 950 ℃/10 min条件下不同Co元素含量非晶钎料钎焊接头断裂路径
Figure 13. Fracture path of brazed joints with different Co content filler metals at 950 ℃/10 min. (a) 0%; (b) 1.56%; (c) 3.12%; (d) 4.68%; (e) 6.24%
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图 14 使用不同钎料钎焊接头断口形貌
Figure 14. Fracture morphology of brazed joints. (a) Ti43.76Zr12.50Cu35.93Ni6.25Co1.56; (b) Ti43.76Zr12.50Cu34.37Ni6.25Co3.12
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图 15 使用不同钎料钎焊接头断口XRD图谱
Figure 15. XRD patterns of fracture surfaces. (a) Ti43.76Zr12.50Cu35.93Ni6.25Co1.56; (b) Ti43.76Zr12.50Cu34.37Ni6.25Co3.12
表 1 母材化学成分(质量分数，%)
Table 1 Chemical compositions of base metals
母材 Al V Cr Ni Mo Mn Fe Ti TC4 5.9 3.6 — — — — — 余量 316L — — 16.5 10.2 2.0 1.3 余量 — 
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表 2 钎料的固相线温度(Tm)和液相线温度(Tl)
Table 2 Solidus temperature and liquidus temperature of filler metals
钎料 固相线
温度
Tm/℃液相线
温度
Tl/℃熔化温度
区间
Tl ~ Tm/℃Ti43.76Zr12.50Cu37.49Ni6.25Co0 847 862 15 Ti43.76Zr12.50Cu35.93Ni6.25Co1.56 843 855 12 Ti43.76Zr12.50Cu34.37Ni6.25Co3.12 849 872 23 Ti43.76Zr12.50Cu32.81Ni6.25Co4.68 850 864 14 Ti43.76Zr12.50Cu31.25Ni6.25Co6.24 854 873 19
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表 3 图6中标记位置的EPMA点元素分析结果(原子分数，%)
Table 3 EPMA analysis results of the marked locations in Fig. 6
点 Ti Cu Zr Ni Co Al V Fe Cr 可能相 A 85.6 0.8 0.3 0.1 — 11.3 1.6 0.2 — α-Ti B 75.8 4.6 0.6 1.4 0.3 7.2 5.8 3.9 0.6 β-Ti C 66.1 23.1 2.5 2.3 0.2 1.9 1.1 2.1 0.8 Ti2Cu D 72.6 7.0 2.8 1.4 0.3 4.5 2.7 6.2 2.5 β-Ti E 40.8 25.0 15.8 4.4 0.4 5.3 1.3 5.4 1.7 (Ti, Zr)2(Cu, Ni) F 63.0 27.9 3.7 2.6 0.2 0.8 0.4 1.3 0.2 Ti2Cu G 50.8 22.0 2.2 3.9 0.9 2.5 1.0 14.3 2.5 Ti2(Cu, Ni) + TiFe H 32.0 0.9 0.9 4.0 0.4 0.5 0.3 52.4 8.5 (Fe, Cr)2Ti I 3.9 0.6 — 3.4 0.3 0.1 0.8 59.1 31.8 α-(Fe, Cr) + τ J 1.0 0.3 — 9.3 0.5 — 0.1 70.8 18.0 γ-(Fe, Ni) + σ
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表 4 图14中标记位置的EDS点元素分析结果(原子分数，%)
Table 4 EDS analysis results of the marked locations in Fig. 14
点 Ti Cu Zr Ni Co Al V Fe Cr 可能相 A 48.4 25.4 5.7 4.8 1.3 2.7 0.7 9.8 1.3 Ti2Cu B 53.8 25.2 11.0 2.8 0.2 3.2 0.4 2.9 0.6 (Ti, Zr)2(Cu, Ni) C 48.1 24.7 13.9 3.8 0.4 3.4 0.7 3.9 1.2 (Ti, Zr)2(Cu, Ni) D 30.8 0.7 2.1 3.4 0.6 1.1 0.4 50.5 10.5 TiFe2 E 48.5 21.7 3.2 3.8 1.3 3.7 0.7 14.9 2.4 Ti2(Cu, Ni) + TiFe F 48.3 23.6 3.5 5.2 1.2 2.3 — 13.9 2.0 Ti2(Cu, Ni) + TiFe G 58.1 12.1 10.2 3.4 0.8 6.5 1.9 5.6 1.6 (Ti, Zr)2(Cu, Ni) H 49.1 18.9 2.0 7.1 2.6 2.6 0.5 15.3 1.9 Ti2(Cu, Ni) + TiFe I 49.9 19.1 2.7 5.7 2.6 3.5 0.6 14.2 1.7 Ti-Cu-Fe J 11.5 0.4 0.7 2.9 0.3 0.7 0.6 57.0 26.0 FeCr K 38.2 5.6 1.3 5.4 1.5 1.6 0.3 36.9 9.3 TiFe L 47.9 19.4 3.0 6.0 2.4 2.9 0.3 16.0 2.2 Ti-Cu-Fe
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