电子封装无铅钎料界面反应研究
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摘要
随着微电子封装领域向互连材料无铅化的方向发展及电子产品向小型化、多功能化的方向迈进，互连焊点的服役可靠性引起了人们的广泛关注。而互连焊点的界面反应是影响焊点可靠性最关键的因素，因此研究无铅钎料的界面反应是非常必要的。
本文首先研究了添加Cu质点的Sn-9Zn复合钎料/Cu基体的界面反应；其次对Sn-Cu基钎料中添加微量合金元素Ti和Ni对界面反应的影响进行了研究，同时也实验研究了低Ag无铅钎料和不同表面处理的焊盘的界面反应；最后对外加电流载荷对无铅焊点界面IMC的生长动力学影响及力学性能损伤进行了探讨。
实验结果表明：1）在Sn9-Zn钎料中添加Cu质点，能有效抑制Sn-9Zn/Cu焊点界面IMC（Cu_5Zn_8）的生长速率，同时焊点内的Cu质点和单质Zn反应，原位转化为Cu-Zn金属间化合物，从而减少了焊点内单质Zn的含量。在钎料中添加的Cu质点越多，界面IMC的生长速率下降得越多。由于在钎焊过程（液-固反应）焊点界面的IMC受到抑制，并且焊点内的Cu质点也消耗了大量单质Zn，因此在时效过程（固-固反应），界面IMC的生长同样受到抑制。2）在Sn-0.7Cu钎料中添加0.008wt%Ti合金元素，可降低Sn-0.7Cu/Cu焊点界面IMC的生长速率。但是，由于在界面IMC中没有检测到Ti的存在，表明Ti并没有参与界面反应。而IMC生长速率降低的原因是Ti的加入降低了界面IMC的形核率，使得IMC晶粒尺寸增加，晶界面积减少，从而导致扩散组元（Cu和Sn）晶间扩散速率减小。另一方面，由于钎料中添加的Ti极为微量，在现有实验条件下，没有检测到钎料中Ti的金属间化合物的存在，这预示Ti原子可能固溶于β-Sn相中或存在于β-Sn相的晶界之间。3）在Sn_(0.8)Ag_(0.5)Cu_2Bi钎料中添加0.05wt%Ni合金元素，其和Cu基体钎焊时的界面反应产物为(Cu,Ni)_6Sn_5，Ni的含量范围为3-4at%。由于(Cu,Ni)_6Sn_5相具有比Cu_6Sn_5相更为复杂的相结构，因此时效过程中界面IMC的生长得到抑制。通过实验计算，其激活能为111.62kJ/mol，大大高于Sn_(3.0)Ag_(0.5)Cu/Cu焊点界面IMC的激活能（75.03kJ/mol）。4）对于Sn_(0.3)Ag_(0.7)Cu钎料和OSP及HASL焊盘的液-固界面反应，其界面IMC为贝状Cu_6Sn_5相；而对于Sn_(0.3)Ag_(0.7)Cu钎料和/ElectrolyticNi/Au及ENIG焊盘来说，其界面IMC为层状和块状的(Cu,Ni)_6Sn_5+针状的(Ni,Cu)_3Sn_4。Sn_(0.3)Ag_(0.7)Cu/ENIG焊点的固-固反应，随着温度和时间的增加，针状(Ni,Cu)_3Sn_4逐渐减少直至最后消失，层状的(Cu,Ni)_6Sn_5增厚；而对于Sn_(0.3)Ag_(0.7)Cu/OSP焊点，其界面IMC－贝状Cu_6Sn_5逐渐变得平整，同时IMC按抛物线规律逐渐增厚。5）Sn3.0Ag0.5Cu/Cu焊点在电流载荷作用下，界面IMC的生长显现明显的极性效应。阳极界面IMC随时间的增加不断增厚，阴极不断减薄，并且阳极IMC的生长动力学符合抛物线生长规律，受扩散机制控制。阴极界面IMC的溶解虽然也符合抛物线规律，但存在一个阴极临界厚度。当阴极的原始厚度大于临界厚度时（电流加载初期），阴极IMC按抛物线规律溶解；当IMC的厚度达到临界厚度时，IMC的厚度几乎不变。另外，电迁移效应将对焊点的力学性能造成极大损伤。
Along with the development towards lead-free interconnection materials inmicro-electronic packaging industry and the progress towards miniaturization andmulti-functionalization for electronic products, the reliability issues of the interconnectionsolder joints as service have aroused the wide attention. However, the interfacial reactionbetween lead-free solder and substrate (including liquid-solid and solid-solid reaction) is themost key issue for the reliability of lead-free solder joint, so, it is necessary to research theinterfacial reaction mechanism for lead-free solder joints.
Firstly, the interfacial reaction between Sn-9Zn solder adding Cu-particle and Cusubstrate was researched in this work. The experimental results show that the growth rate ofthe interfacial IMC (Cu_5Zn_8) in the solder joints can be fully suppressed by addingCu-particle in the solder, meanwhile, Zn phase inside the solder joint is in situ transformedinto Cu-Zn intermetallic compounds due to its reaction with Cu-particle, resulting in Zn phasedecreasing. Since the growth rate of the interfacial IMC of the solder/Cu-substrate isobviously lower than the solder/Cu-particle, it is concluded that Cu-particle is able to“capture” the more Zn atom than Cu-substrate. This can be explained as that the quantities ofthe liquid solder reacting with Cu-particle are the more than Cu-substrate in the now reactionsystem by means of Dybkov’s interfacial reaction theory.
Secondly, the effect of adding trace alloy elements Ti and Ni in Sn base solder on theinterfacial reaction was explored. The results indicate that the growth rate of the interfacialIMC between Sn-0.7Cu solder and Cu substrate can be decreased in some extent, and it is alsoobserved that the IMC grain size increases when0.008wt%Ti is added in the solder as alloyelement. However, since Ti element is not detected in the interfacial IMC, this concluded thatthere is not any reaction between Ti and other constituents forming the IMC. So, themechanism-controlled depressing the IMC growth rate may be considered that the boundarydiffusion of the constituents Cu and Sn is restrained due to decreasing the nucleation of theinterfacial IMC as adding Ti in the solder, resulting in the grain size increasing, meanwhile,the boundary area decreasing. When0.05wt%Ni is added in Sn_(0.8)Ag_(0.5)Cu_2Bi solder as alloy element, the interfacial reaction IMC between the solder and Cu substrate is (Cu,Ni)_6Sn_5assoldering, and Ni content in the IMC is about3-4at%by EDS. Since the (Cu,Ni)_6Sn_5configuration is more complex than Cu_6Sn_5, its growth rate is depressed as isothermal aging.The (Cu,Ni)_6Sn_5growth activation energy calculated by experimental data is about111.62kJ/mol, and it is more larger than Cu_6Sn_5(about75.03kJ/mol).
Additionally, the interfacial reactions between Sn_(0.3)Ag_(0.7)Cu solder and dissimilar padsfinish (including OSP, HASL, Electrolytic Ni/Au and ENIG) were comparatively investigated.It is presented that scallop-shaped Cu_6Sn_5are formed between the solder and OSP as well asHASL pads finish as soldering, however, the interfacial IMC with Electrolytic Ni/Au andENIG pads finish are composed of layer-shaped and dollop-shaped (Cu,Ni)_6Sn_5as well asneedle-shaped (Ni,Cu)_3Sn_4. During isothermal aging, the needle-shaped (Ni,Cu)_3Sn_4gradually reduce till completely vanish and the thickness of layer-shaped (Cu,Ni)_6Sn_5,simultaneously, increases with aging time increasing. It is concluded that Cu atom in thesubstrate participates in the interfacial reaction and its diffusive rate through Ni layerdominates the IMC growth rate, therefore, the needle-shaped (Ni,Cu)_3Sn_4more slowly reduceas the Ni layer is more thick.
Finally, the growth kinetics of the interfacial IMC of Sn_(3.0)Ag_(0.5)Cu/Cu solder joints wasalso explored under stressing electric current. It is indicated that the evolution on theinterfacial IMC between the solder and Cu substrate presents an obvious polarity effect atcathode and anode. The growth rate of the interfacial IMC is strengthened at anode andinhibited at cathode, and its growth kinetics at anode accords with parabolic relationship withstressing time. Although the dissolution rate of the interfacial IMC at cathode also isaccordance with parabolic rule, the IMC thickness exist a threshold value. When the IMCthickness is larger than the threshold value (early stage), the IMC dissolution followsparabolic rule, however, as the IMC thickness is equal to the threshold value, it is hardlychanged. This concludes that the driven forces acted on the diffusive atoms at cathode takebalance, namely, electronic wind force is equal to chemical potential energy.
本文首先研究了添加Cu质点的Sn-9Zn复合钎料/Cu基体的界面反应；其次对Sn-Cu基钎料中添加微量合金元素Ti和Ni对界面反应的影响进行了研究，同时也实验研究了低Ag无铅钎料和不同表面处理的焊盘的界面反应；最后对外加电流载荷对无铅焊点界面IMC的生长动力学影响及力学性能损伤进行了探讨。
实验结果表明：1）在Sn9-Zn钎料中添加Cu质点，能有效抑制Sn-9Zn/Cu焊点界面IMC（Cu_5Zn_8）的生长速率，同时焊点内的Cu质点和单质Zn反应，原位转化为Cu-Zn金属间化合物，从而减少了焊点内单质Zn的含量。在钎料中添加的Cu质点越多，界面IMC的生长速率下降得越多。由于在钎焊过程（液-固反应）焊点界面的IMC受到抑制，并且焊点内的Cu质点也消耗了大量单质Zn，因此在时效过程（固-固反应），界面IMC的生长同样受到抑制。2）在Sn-0.7Cu钎料中添加0.008wt%Ti合金元素，可降低Sn-0.7Cu/Cu焊点界面IMC的生长速率。但是，由于在界面IMC中没有检测到Ti的存在，表明Ti并没有参与界面反应。而IMC生长速率降低的原因是Ti的加入降低了界面IMC的形核率，使得IMC晶粒尺寸增加，晶界面积减少，从而导致扩散组元（Cu和Sn）晶间扩散速率减小。另一方面，由于钎料中添加的Ti极为微量，在现有实验条件下，没有检测到钎料中Ti的金属间化合物的存在，这预示Ti原子可能固溶于β-Sn相中或存在于β-Sn相的晶界之间。3）在Sn_(0.8)Ag_(0.5)Cu_2Bi钎料中添加0.05wt%Ni合金元素，其和Cu基体钎焊时的界面反应产物为(Cu,Ni)_6Sn_5，Ni的含量范围为3-4at%。由于(Cu,Ni)_6Sn_5相具有比Cu_6Sn_5相更为复杂的相结构，因此时效过程中界面IMC的生长得到抑制。通过实验计算，其激活能为111.62kJ/mol，大大高于Sn_(3.0)Ag_(0.5)Cu/Cu焊点界面IMC的激活能（75.03kJ/mol）。4）对于Sn_(0.3)Ag_(0.7)Cu钎料和OSP及HASL焊盘的液-固界面反应，其界面IMC为贝状Cu_6Sn_5相；而对于Sn_(0.3)Ag_(0.7)Cu钎料和/ElectrolyticNi/Au及ENIG焊盘来说，其界面IMC为层状和块状的(Cu,Ni)_6Sn_5+针状的(Ni,Cu)_3Sn_4。Sn_(0.3)Ag_(0.7)Cu/ENIG焊点的固-固反应，随着温度和时间的增加，针状(Ni,Cu)_3Sn_4逐渐减少直至最后消失，层状的(Cu,Ni)_6Sn_5增厚；而对于Sn_(0.3)Ag_(0.7)Cu/OSP焊点，其界面IMC－贝状Cu_6Sn_5逐渐变得平整，同时IMC按抛物线规律逐渐增厚。5）Sn3.0Ag0.5Cu/Cu焊点在电流载荷作用下，界面IMC的生长显现明显的极性效应。阳极界面IMC随时间的增加不断增厚，阴极不断减薄，并且阳极IMC的生长动力学符合抛物线生长规律，受扩散机制控制。阴极界面IMC的溶解虽然也符合抛物线规律，但存在一个阴极临界厚度。当阴极的原始厚度大于临界厚度时（电流加载初期），阴极IMC按抛物线规律溶解；当IMC的厚度达到临界厚度时，IMC的厚度几乎不变。另外，电迁移效应将对焊点的力学性能造成极大损伤。
Along with the development towards lead-free interconnection materials inmicro-electronic packaging industry and the progress towards miniaturization andmulti-functionalization for electronic products, the reliability issues of the interconnectionsolder joints as service have aroused the wide attention. However, the interfacial reactionbetween lead-free solder and substrate (including liquid-solid and solid-solid reaction) is themost key issue for the reliability of lead-free solder joint, so, it is necessary to research theinterfacial reaction mechanism for lead-free solder joints.
Firstly, the interfacial reaction between Sn-9Zn solder adding Cu-particle and Cusubstrate was researched in this work. The experimental results show that the growth rate ofthe interfacial IMC (Cu_5Zn_8) in the solder joints can be fully suppressed by addingCu-particle in the solder, meanwhile, Zn phase inside the solder joint is in situ transformedinto Cu-Zn intermetallic compounds due to its reaction with Cu-particle, resulting in Zn phasedecreasing. Since the growth rate of the interfacial IMC of the solder/Cu-substrate isobviously lower than the solder/Cu-particle, it is concluded that Cu-particle is able to“capture” the more Zn atom than Cu-substrate. This can be explained as that the quantities ofthe liquid solder reacting with Cu-particle are the more than Cu-substrate in the now reactionsystem by means of Dybkov’s interfacial reaction theory.
Secondly, the effect of adding trace alloy elements Ti and Ni in Sn base solder on theinterfacial reaction was explored. The results indicate that the growth rate of the interfacialIMC between Sn-0.7Cu solder and Cu substrate can be decreased in some extent, and it is alsoobserved that the IMC grain size increases when0.008wt%Ti is added in the solder as alloyelement. However, since Ti element is not detected in the interfacial IMC, this concluded thatthere is not any reaction between Ti and other constituents forming the IMC. So, themechanism-controlled depressing the IMC growth rate may be considered that the boundarydiffusion of the constituents Cu and Sn is restrained due to decreasing the nucleation of theinterfacial IMC as adding Ti in the solder, resulting in the grain size increasing, meanwhile,the boundary area decreasing. When0.05wt%Ni is added in Sn_(0.8)Ag_(0.5)Cu_2Bi solder as alloy element, the interfacial reaction IMC between the solder and Cu substrate is (Cu,Ni)_6Sn_5assoldering, and Ni content in the IMC is about3-4at%by EDS. Since the (Cu,Ni)_6Sn_5configuration is more complex than Cu_6Sn_5, its growth rate is depressed as isothermal aging.The (Cu,Ni)_6Sn_5growth activation energy calculated by experimental data is about111.62kJ/mol, and it is more larger than Cu_6Sn_5(about75.03kJ/mol).
Additionally, the interfacial reactions between Sn_(0.3)Ag_(0.7)Cu solder and dissimilar padsfinish (including OSP, HASL, Electrolytic Ni/Au and ENIG) were comparatively investigated.It is presented that scallop-shaped Cu_6Sn_5are formed between the solder and OSP as well asHASL pads finish as soldering, however, the interfacial IMC with Electrolytic Ni/Au andENIG pads finish are composed of layer-shaped and dollop-shaped (Cu,Ni)_6Sn_5as well asneedle-shaped (Ni,Cu)_3Sn_4. During isothermal aging, the needle-shaped (Ni,Cu)_3Sn_4gradually reduce till completely vanish and the thickness of layer-shaped (Cu,Ni)_6Sn_5,simultaneously, increases with aging time increasing. It is concluded that Cu atom in thesubstrate participates in the interfacial reaction and its diffusive rate through Ni layerdominates the IMC growth rate, therefore, the needle-shaped (Ni,Cu)_3Sn_4more slowly reduceas the Ni layer is more thick.
Finally, the growth kinetics of the interfacial IMC of Sn_(3.0)Ag_(0.5)Cu/Cu solder joints wasalso explored under stressing electric current. It is indicated that the evolution on theinterfacial IMC between the solder and Cu substrate presents an obvious polarity effect atcathode and anode. The growth rate of the interfacial IMC is strengthened at anode andinhibited at cathode, and its growth kinetics at anode accords with parabolic relationship withstressing time. Although the dissolution rate of the interfacial IMC at cathode also isaccordance with parabolic rule, the IMC thickness exist a threshold value. When the IMCthickness is larger than the threshold value (early stage), the IMC dissolution followsparabolic rule, however, as the IMC thickness is equal to the threshold value, it is hardlychanged. This concludes that the driven forces acted on the diffusive atoms at cathode takebalance, namely, electronic wind force is equal to chemical potential energy.
引文
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