稀土Pr和Nd对SnAgCu无铅钎料组织与性能影响研究
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摘要
随着电子封装技术的发展以及无铅化进程的推进，无铅钎料的研究已经成为电子封装领域的重要课题之一。SnAgCu系钎料合金由于其较优的综合性能，被认为是电子行业中最具潜力替代SnPb钎料的无铅钎料之一，但其润湿性能、凝固特性以及服役过程中的组织稳定性等仍存在一些不足，SnAgCu钎料的高Sn含量、较高钎焊温度使得其焊点内部金属间化合物的生长相比SnPb钎料要复杂得多。微量元素合金化是获得高性能无铅钎料的有效途径之一，本论文通过添加微量的稀土Pr和Nd元素来改善Sn3.8Ag0.7Cu无铅钎料的不足之处，系统地研究了不同含量(0~0.5wt.%)Pr和Nd的添加对SnAgCu钎料性能以及组织的影响，并对Pr和Nd元素的作用机制进行了探讨。
采用润湿平衡法研究了不同含量Pr和Nd的添加对SnAgCu钎料润湿性能的影响。研究结果表明，适量稀土元素Pr和Nd的添加可以明显改善SnAgCu钎料的润湿性能，当稀土元素Pr和Nd的添加量分别为0.05wt.%时，钎料具有最佳的润湿性能，250℃试验条件下，SnAgCu-0.05Pr以及SnAgCu-0.05Nd钎料相比SnAgCu钎料润湿力分别提高了6.7%以及5.5%，润湿时间分别降低了14.5%以及10.0%。由于Pr和Nd为表面活性元素，适量添加可以降低液态钎料表面张力，改善钎料的润湿性能；但添加过量则会由于稀土元素的氧化恶化钎料的润湿性能。
研究了SnAgCu-xRE(x=0,0.05,0.50wt.%)钎料的熔化温度以及凝固所需过冷度，微量Pr和Nd的添加对SnAgCu钎料的熔化温度没有明显的影响，但可以显著降低SnAgCu钎料的凝固过冷度，SnAgCu、SnAgCu-0.05Pr以及SnAgCu-0.5Pr钎料的凝固过冷度分别为20.6℃、5.0℃以及5.5℃，因而可以降低SnAgCu焊点中初晶Ag3Sn的形成几率。凝固过程中，Pr和Nd可以优先与Sn反应，以Sn-RE化合物形式优先析出，为钎料的凝固提供形核质点，促进钎料的凝固。当稀土元素Pr和Nd的含量在0.05wt.%左右时，SnAgCu钎料基体组织得到最大程度的优化，当含量超过0.1wt.%时，钎料中会出现少量的稀土相RESn3相。
采用纳米压痕试验方法对SnAgCu-xRE(x=0,0.05,0.50wt.%)钎料室温条件下的蠕变应力指数n进行了研究。SnAgCu、SnAgCu-0.05Pr、SnAgCu-0.5Pr、SnAgCu-0.05Nd以及SnAgCu-0.5Nd的蠕变应力指数值n分别为8.79、10.19、9.26、10.97以及9.84，Pr和Nd的添加使得SnAgCu钎料的蠕变应力指数n值明显增加，表明Pr和Nd的添加可以显著增强SnAgCu钎料的抗蠕变能力，SnAgCu钎料抗蠕变能力的增强主要依赖于Ag3Sn粒子强化作用。
研究发现，Pr或Nd的添加可以显著提高SnAgCu微焊点再流焊以及时效过程中力学性能，再流焊条件下，SnAgCu-0.05Pr以及SnAgCu-0.05Nd微焊点剪切力相比SnAgCu分别增加了19.4%以及23.6%；随着时效的进行，微焊点力学性能下降，但SnAgCu-0.05RE微焊点始终具有最高的力学性能，时效1440h后，SnAgCu-0.05Pr以及SnAgCu-0.05Nd微焊点力学性能相比SnAgCu焊点分别提高了37.3%以及46.0%。Pr和Nd的添加明显降低了SnAgCu/Cu焊点时效过程中界面化合物总厚度生长速率，有利于焊点力学性能的保持，但对焊点Cu3Sn界面层的生长没有明显的影响。部分稀土相在界面层Cu6Sn5表面形核并长大，部分Cu6Sn5/钎料界面由Cu6Sn5/RESn3界面所取代，抑制了Cu6Sn5/钎料界面处反应6Cu+5Sn→Cu6Sn5的进行，因而抑制了Cu6Sn5界面层的生长；当Pr和Nd的添加量过多时，裸露于空气中的稀土相由于氧化呈现脆性特征，稀土元素对焊点界面层生长抑制的有利效果被弱化。
采用深腐蚀方法对焊点内部化合物三维形貌进行了研究分析。发现，Pr和Nd的添加可以降低SnAgCu焊点Cu6Sn5界面处初晶Ag3Sn的形成几率，初晶Ag3Sn具有较大的尺寸，对焊点力学性能整体性会产生不利的影响。时效条件下，界面层Cu6Sn5晶粒存在横向粗化以及纵向延长生长两种生长行为；初晶Ag3Sn化合物的形貌以及尺寸均发生了退化现象，焊点内部形成的纳米Ag3Sn粒子易于在初晶Ag3Sn表面吸附。Ag3Sn颗粒的存在对Cu6Sn5界面层向焊点内部迁移生长起到钉扎的效果，从而降低了Cu6Sn5界面层的迁移速率，Pr和Nd的添加可以使得SnAgCu焊点内部Ag3Sn颗粒的体积分数增加，因而可以降低焊点界面层的迁移速率。
SnAgCu钎料中过量Pr和Nd的添加会引发稀土相表面Sn须的生长，SnAgCu-0.1RE合金置于室温条件下时效6个月后，稀土相表面未见有可见尺寸Sn须的生长现象；SnAgCu-0.5RE以及Sn-RE合金室温时效24h后，表面就会出现明显的Sn须生长现象。稀土相表面Sn须的生长主要是由于裸露于空气中的稀土相氧化所导致，氧化过程过程中产生的内应力以及释放的自由Sn原子为Sn须的生长提供驱动力以及生长源。Sn须生长主要受稀土元素含量、稀土相表面微裂纹形貌以及Sn须根部微区应力的共同影响。
As fast development of electronic packaging technology and the inevitable trend of lead-freesoldering, the research focusing on lead-free solder alloys becomes more and more important in theelectronic industry. SnAgCu solder is considered as the best one to substitute for Pb-containingsolders because of their acceptable comprehensive property. However, they still have some problemsfor widely industrial application compare to conventional SnPb alloy, such as microstructural stability,insufficient wettability and large solidification undercooling. Moreover, the growth of intermetalliccompounds in the SnAgCu solder joints is more complicated than that of SnPb due to the higher Sncontent and soldering temperature of SnAgCu alloys. Microalloying is an effective way to improvethe properties of the solder alloys. To improve these drawbacks, rare-earth elements RE (RE=Pr, Nd)were selected to improve the properties and microstructures of Sn3.8Ag0.7Cu solder alloy. Thisdissertation systematically studied the effects of different amounts (0~0.5wt.%) of Pr and Ndadditions on the microstructures and properties of Sn3.8Ag0.7Cu alloy. Moreover, the mechanism ofthe effects of Pr and Nd on the microstructures and properties of SnAgCu solder was also discussed.
The wetting balance method was used to evaluate the wettability of Sn3.8Ag0.7Cu-xRE solders,and the results indicated that trace amount of Pr and Nd addition could obviously improve thewettability of the SnAgCu solder, which the optimal wettability was achieved as the RE content isabout0.05wt.%due to the lower surface tension caused by RE elements. When measured at250℃,the wetting force of of SnAgCu solder was increased by6.7%and5.5%with0.05%Pr or0.05%Ndand the wetting time of SnAgCu solder was descreased by14.5%and10.0%, respectively under thesame condition. However, an excessive amount of RE addition into the solder would deteriorate thewettability due to the oxidization of the RE elements.
The effects of RE additions on the melting and solidification behavior of SnAgCu solder wereinvestigated and the melting point of SnAgCu alloy changed little with the incorporation of REelements. However, the RE additions reduced the amount of solidification undercooling of SnAgCusolder thus reduced the probability of primary Ag3Sn phase formation. The undercooling of SnAgCu,SnAgCu-0.05Pr and SnAgCu-0.5Pr solder was20.6,5.0and5.5℃, respectively. During solidification,Pr and Nd atoms preferentially reacted with Sn atoms to form RESn3compound, the primary RESn3compounds played a role as the nucleation sites thus promoted the solidification of the solder alloy.The microstructure of SnAgCu-0.05RE alloy was finer and more uniform compared with that of other solder alloys. However, RESn3compounds were found in the solder as RE was added up to0.1wt.%.
Nanoindentation was adapted to characterize the creep stress exponent n of SnAgCu-xRE solderalloys. Both RE bearing solders exhibited larger n than that of SnAgCu solder, with a creep stressexponent8.79for SnAgCu,10.19for SnAgCu-0.05Pr,9.26for SnAgCu-0.5Pr,10.97forSnAgCu-0.05Nd and9.84for SnAgCu-0.5Nd. It can be concluded that RE-bearing solder alloysperform better creep resistance than SnAgCu solder, which can be atttributed to the strengthen effectof Ag3Sn particles.
The results showed that the mechanical property of SnAgCu solder joint were improved with Prand Nd addition, the maxium shear force was obtained with about0.05%Pr or Nd addition andexhibited a19.4%and23.6%increase compare with that of SnAgCu solder joint, respectively. Duringthermal aging process, the shear strength of all solder joints decreased with the increase of aging time,the SnAgCu-0.05RE solder joint exhibited the highest shear force all through the aging process. Afteraging for1440h, the shear force of SnAgCu-0.05Pr and SnAgCu-0.05Nd were37.3%and46.0%higher than that of SnAgCu solder joint. Trace amounts of Pr and Nd additions suppressed the growthof Cu6Sn5layer, but had little influence on Cu3Sn layer. Part of the Cu6Sn5/solder interface wasreplaced by Cu6Sn5/RESn3interface, the existence of RESn3compounds at the interface would inhibitthe reaction of6Cu+5Sn→Cu6Sn5that take place at Cu6Sn5/solder interface thus restrain the growthof Cu6Sn5layer. With an excessive amount of RE addition, the RESn3phase exposed in room ambienttransformed into brittle oxide. Consequently, the beneficial effect due to the suppression of interfaciallayer compounds was weakened.
Three-dimensional morphology of the intermetallic compounds (IMCs) in the solder joints wasstudied by deep etching method. The results showed that the Pr and Nd addition could reduce theprobability of primary Ag3Sn phase formation in the SnAgCu solder joint, the existence of primaryAg3Sn plates with large size had an adverse influence on the mechanical property of the joint. Duringaging process, the Cu6Sn5grains at the interface showed both horizontal coarsening and longitudinalgrowth. After aging, the feature distinctions of primary Ag3Sn compound were inclined to be vague,Ag3Sn nano-particles adsorbed on the primary Ag3Sn compound would retard the morphologyevalution of primary Ag3Sn compound. It could be considered as that the presence of Ag3Sn particlesat the surface of Cu6Sn5layer could retard the migration of Cu6Sn5layer. The addition of Pr and Ndwould increase the volume fraction of Ag3Sn particles in the solder joint thus inhibit the growth of theinterfacial layer.
When an excessive amount of RE was added in SnAgCu solder alloy, the risk of forming Sn whisker was greatly increased due to the induced compressive stress and released Sn atoms caused byoxidation of RESn3compound. It was found that there was no Sn whisker with visible size growthoccurred on the surface of SnAgCu-0.1RE samples after room temperature storage for six months.However, SnAgCu-0.5RE and Sn-RE alloys showed obvious Sn whisker growth after roomtemperature storage for24h. It can be concluded that the growth of Sn whisker was mainly resulted inthe RE amount, the micro-cracks shape and the local stress filed in Sn whisker root area.
采用润湿平衡法研究了不同含量Pr和Nd的添加对SnAgCu钎料润湿性能的影响。研究结果表明，适量稀土元素Pr和Nd的添加可以明显改善SnAgCu钎料的润湿性能，当稀土元素Pr和Nd的添加量分别为0.05wt.%时，钎料具有最佳的润湿性能，250℃试验条件下，SnAgCu-0.05Pr以及SnAgCu-0.05Nd钎料相比SnAgCu钎料润湿力分别提高了6.7%以及5.5%，润湿时间分别降低了14.5%以及10.0%。由于Pr和Nd为表面活性元素，适量添加可以降低液态钎料表面张力，改善钎料的润湿性能；但添加过量则会由于稀土元素的氧化恶化钎料的润湿性能。
研究了SnAgCu-xRE(x=0,0.05,0.50wt.%)钎料的熔化温度以及凝固所需过冷度，微量Pr和Nd的添加对SnAgCu钎料的熔化温度没有明显的影响，但可以显著降低SnAgCu钎料的凝固过冷度，SnAgCu、SnAgCu-0.05Pr以及SnAgCu-0.5Pr钎料的凝固过冷度分别为20.6℃、5.0℃以及5.5℃，因而可以降低SnAgCu焊点中初晶Ag3Sn的形成几率。凝固过程中，Pr和Nd可以优先与Sn反应，以Sn-RE化合物形式优先析出，为钎料的凝固提供形核质点，促进钎料的凝固。当稀土元素Pr和Nd的含量在0.05wt.%左右时，SnAgCu钎料基体组织得到最大程度的优化，当含量超过0.1wt.%时，钎料中会出现少量的稀土相RESn3相。
采用纳米压痕试验方法对SnAgCu-xRE(x=0,0.05,0.50wt.%)钎料室温条件下的蠕变应力指数n进行了研究。SnAgCu、SnAgCu-0.05Pr、SnAgCu-0.5Pr、SnAgCu-0.05Nd以及SnAgCu-0.5Nd的蠕变应力指数值n分别为8.79、10.19、9.26、10.97以及9.84，Pr和Nd的添加使得SnAgCu钎料的蠕变应力指数n值明显增加，表明Pr和Nd的添加可以显著增强SnAgCu钎料的抗蠕变能力，SnAgCu钎料抗蠕变能力的增强主要依赖于Ag3Sn粒子强化作用。
研究发现，Pr或Nd的添加可以显著提高SnAgCu微焊点再流焊以及时效过程中力学性能，再流焊条件下，SnAgCu-0.05Pr以及SnAgCu-0.05Nd微焊点剪切力相比SnAgCu分别增加了19.4%以及23.6%；随着时效的进行，微焊点力学性能下降，但SnAgCu-0.05RE微焊点始终具有最高的力学性能，时效1440h后，SnAgCu-0.05Pr以及SnAgCu-0.05Nd微焊点力学性能相比SnAgCu焊点分别提高了37.3%以及46.0%。Pr和Nd的添加明显降低了SnAgCu/Cu焊点时效过程中界面化合物总厚度生长速率，有利于焊点力学性能的保持，但对焊点Cu3Sn界面层的生长没有明显的影响。部分稀土相在界面层Cu6Sn5表面形核并长大，部分Cu6Sn5/钎料界面由Cu6Sn5/RESn3界面所取代，抑制了Cu6Sn5/钎料界面处反应6Cu+5Sn→Cu6Sn5的进行，因而抑制了Cu6Sn5界面层的生长；当Pr和Nd的添加量过多时，裸露于空气中的稀土相由于氧化呈现脆性特征，稀土元素对焊点界面层生长抑制的有利效果被弱化。
采用深腐蚀方法对焊点内部化合物三维形貌进行了研究分析。发现，Pr和Nd的添加可以降低SnAgCu焊点Cu6Sn5界面处初晶Ag3Sn的形成几率，初晶Ag3Sn具有较大的尺寸，对焊点力学性能整体性会产生不利的影响。时效条件下，界面层Cu6Sn5晶粒存在横向粗化以及纵向延长生长两种生长行为；初晶Ag3Sn化合物的形貌以及尺寸均发生了退化现象，焊点内部形成的纳米Ag3Sn粒子易于在初晶Ag3Sn表面吸附。Ag3Sn颗粒的存在对Cu6Sn5界面层向焊点内部迁移生长起到钉扎的效果，从而降低了Cu6Sn5界面层的迁移速率，Pr和Nd的添加可以使得SnAgCu焊点内部Ag3Sn颗粒的体积分数增加，因而可以降低焊点界面层的迁移速率。
SnAgCu钎料中过量Pr和Nd的添加会引发稀土相表面Sn须的生长，SnAgCu-0.1RE合金置于室温条件下时效6个月后，稀土相表面未见有可见尺寸Sn须的生长现象；SnAgCu-0.5RE以及Sn-RE合金室温时效24h后，表面就会出现明显的Sn须生长现象。稀土相表面Sn须的生长主要是由于裸露于空气中的稀土相氧化所导致，氧化过程过程中产生的内应力以及释放的自由Sn原子为Sn须的生长提供驱动力以及生长源。Sn须生长主要受稀土元素含量、稀土相表面微裂纹形貌以及Sn须根部微区应力的共同影响。
As fast development of electronic packaging technology and the inevitable trend of lead-freesoldering, the research focusing on lead-free solder alloys becomes more and more important in theelectronic industry. SnAgCu solder is considered as the best one to substitute for Pb-containingsolders because of their acceptable comprehensive property. However, they still have some problemsfor widely industrial application compare to conventional SnPb alloy, such as microstructural stability,insufficient wettability and large solidification undercooling. Moreover, the growth of intermetalliccompounds in the SnAgCu solder joints is more complicated than that of SnPb due to the higher Sncontent and soldering temperature of SnAgCu alloys. Microalloying is an effective way to improvethe properties of the solder alloys. To improve these drawbacks, rare-earth elements RE (RE=Pr, Nd)were selected to improve the properties and microstructures of Sn3.8Ag0.7Cu solder alloy. Thisdissertation systematically studied the effects of different amounts (0~0.5wt.%) of Pr and Ndadditions on the microstructures and properties of Sn3.8Ag0.7Cu alloy. Moreover, the mechanism ofthe effects of Pr and Nd on the microstructures and properties of SnAgCu solder was also discussed.
The wetting balance method was used to evaluate the wettability of Sn3.8Ag0.7Cu-xRE solders,and the results indicated that trace amount of Pr and Nd addition could obviously improve thewettability of the SnAgCu solder, which the optimal wettability was achieved as the RE content isabout0.05wt.%due to the lower surface tension caused by RE elements. When measured at250℃,the wetting force of of SnAgCu solder was increased by6.7%and5.5%with0.05%Pr or0.05%Ndand the wetting time of SnAgCu solder was descreased by14.5%and10.0%, respectively under thesame condition. However, an excessive amount of RE addition into the solder would deteriorate thewettability due to the oxidization of the RE elements.
The effects of RE additions on the melting and solidification behavior of SnAgCu solder wereinvestigated and the melting point of SnAgCu alloy changed little with the incorporation of REelements. However, the RE additions reduced the amount of solidification undercooling of SnAgCusolder thus reduced the probability of primary Ag3Sn phase formation. The undercooling of SnAgCu,SnAgCu-0.05Pr and SnAgCu-0.5Pr solder was20.6,5.0and5.5℃, respectively. During solidification,Pr and Nd atoms preferentially reacted with Sn atoms to form RESn3compound, the primary RESn3compounds played a role as the nucleation sites thus promoted the solidification of the solder alloy.The microstructure of SnAgCu-0.05RE alloy was finer and more uniform compared with that of other solder alloys. However, RESn3compounds were found in the solder as RE was added up to0.1wt.%.
Nanoindentation was adapted to characterize the creep stress exponent n of SnAgCu-xRE solderalloys. Both RE bearing solders exhibited larger n than that of SnAgCu solder, with a creep stressexponent8.79for SnAgCu,10.19for SnAgCu-0.05Pr,9.26for SnAgCu-0.5Pr,10.97forSnAgCu-0.05Nd and9.84for SnAgCu-0.5Nd. It can be concluded that RE-bearing solder alloysperform better creep resistance than SnAgCu solder, which can be atttributed to the strengthen effectof Ag3Sn particles.
The results showed that the mechanical property of SnAgCu solder joint were improved with Prand Nd addition, the maxium shear force was obtained with about0.05%Pr or Nd addition andexhibited a19.4%and23.6%increase compare with that of SnAgCu solder joint, respectively. Duringthermal aging process, the shear strength of all solder joints decreased with the increase of aging time,the SnAgCu-0.05RE solder joint exhibited the highest shear force all through the aging process. Afteraging for1440h, the shear force of SnAgCu-0.05Pr and SnAgCu-0.05Nd were37.3%and46.0%higher than that of SnAgCu solder joint. Trace amounts of Pr and Nd additions suppressed the growthof Cu6Sn5layer, but had little influence on Cu3Sn layer. Part of the Cu6Sn5/solder interface wasreplaced by Cu6Sn5/RESn3interface, the existence of RESn3compounds at the interface would inhibitthe reaction of6Cu+5Sn→Cu6Sn5that take place at Cu6Sn5/solder interface thus restrain the growthof Cu6Sn5layer. With an excessive amount of RE addition, the RESn3phase exposed in room ambienttransformed into brittle oxide. Consequently, the beneficial effect due to the suppression of interfaciallayer compounds was weakened.
Three-dimensional morphology of the intermetallic compounds (IMCs) in the solder joints wasstudied by deep etching method. The results showed that the Pr and Nd addition could reduce theprobability of primary Ag3Sn phase formation in the SnAgCu solder joint, the existence of primaryAg3Sn plates with large size had an adverse influence on the mechanical property of the joint. Duringaging process, the Cu6Sn5grains at the interface showed both horizontal coarsening and longitudinalgrowth. After aging, the feature distinctions of primary Ag3Sn compound were inclined to be vague,Ag3Sn nano-particles adsorbed on the primary Ag3Sn compound would retard the morphologyevalution of primary Ag3Sn compound. It could be considered as that the presence of Ag3Sn particlesat the surface of Cu6Sn5layer could retard the migration of Cu6Sn5layer. The addition of Pr and Ndwould increase the volume fraction of Ag3Sn particles in the solder joint thus inhibit the growth of theinterfacial layer.
When an excessive amount of RE was added in SnAgCu solder alloy, the risk of forming Sn whisker was greatly increased due to the induced compressive stress and released Sn atoms caused byoxidation of RESn3compound. It was found that there was no Sn whisker with visible size growthoccurred on the surface of SnAgCu-0.1RE samples after room temperature storage for six months.However, SnAgCu-0.5RE and Sn-RE alloys showed obvious Sn whisker growth after roomtemperature storage for24h. It can be concluded that the growth of Sn whisker was mainly resulted inthe RE amount, the micro-cracks shape and the local stress filed in Sn whisker root area.
引文
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