部分无铅焊料体系的热力学与动力学研究
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摘要
焊接材料在电子封装中起着重要的作用，然而传统的Sn-Pb焊料中的Pb对人类的身体健康和环境造成极大的危害。这一问题已经引起欧美、日本及我国政府的高度重视，并已制定出多项政策来限制含铅焊接材料的使用。无铅焊料的研究已是电子封装领域研究的热点之一。经过近十年有关无铅焊料的研究表明，无铅焊接材料不可能是简单的二元合金，而是由多元素构成的多元合金。目前在研究和开发该材料的过程中，主要是尝试研究法，这消耗了大量的人力和物力。相图热力学与动力学计算在材料的研究设计方面具有重要的指导作用，并且成为研究比较活跃的领域之一。无铅焊料热力学数据库和动力学数据库的建立可以减少大量的无铅焊料设计过程中的实验、减小设计开发成本，并且为界面反应研究提供了一个很有效的工具。
本研究的主要工作是完善已有的无铅焊料设计系统和初步建立无铅焊料动力学数据库。本研究利用电子探针(EPMA：electron probe micro-analyzer)通过合金法和扩散偶法对部分无铅焊料三元系相平衡进行了实验测定；利用差示扫描量热分析(DSC：differential scanning calorimetry)测定了部分相变温度；利用相图计算的CALPHAD(calculation of phase diagrams)方法对无铅焊料部分二元和三元系的相图进行热力学计算，获得整个体系较为精确的相图和合理的热力学参数，从而完善无铅焊接材料热力学数据库。同时，利用DICTRA软件对纯组元和部分二元系的动力学参数进行优化，初步建立无铅焊接材料动力学数据库。本研究的主要内容如下：
(1)基于合金法和扩散偶法实验方法，(a)测定了Sn-Ag-Au三元系在300℃、400℃和500℃的相平衡和部分不变反应的温度；(b)测定了Sn-Au-Bi三元系在200℃、250℃、300℃和400℃的相平衡和部分不变反应温度，结果表明在Sn-Au-Bi三元系有一个三元金属间化合物(ψ)，该ψ相300℃时固溶度范围为Sn_(12．2)Au_(48．8)Bi_(39)到Sn_(13)Au_(49)Bi_(38)(at．％)，熔点为312．7℃。X-射线衍射分析表明ψ相的空间群为P63／mmc，具有和AuSn相类似的结构；(c)测定了Sn-Cu-Ni和Sn-Au-Cu三元系在500℃的相平衡关系，初步确定了500℃的等温截面相图；(d)测定了Ag-Bi-Ni和Cu-Bi-Ni三元系的相平衡，并首次确定了在300℃、400℃和500℃的Ag-Bi-Ni和Cu-Bi-Ni三元系的等温截面相图，确定了Cu-Bi-Ni三元系300℃在Cu-Ni侧存在一个NiBi+fcc(Cu)+fcc(Ni)的三相平衡区；(e)测定了Bi-Ni-Zn体系在300℃、500℃和700℃的相平衡；(f)测定了Sn-Ni二元系和Sn-Bi-Ni三元系部分相平衡，确定Sn-Ni二元系内不存在NiSn相，而是一个固溶范围较大的Ni_3Sn_4相。
(2)利用CALPHAD方法，根据本研究测定的实验数据和文献报道的实验数据，(a)对Sn-Ni、Sn-Ag-Au、Sn-Ag-Ni、Sn-Au-Bi、Ag-Bi-Ni、Cu-Bi-Ni等体系相图进行了热力学计算，其结果与实验数据吻合的较好：(b)对Sn-Cu-Ni和Sn-Au-Cu三元系相图进行了初步的热力学计算，计算结果与实验数据基本是一致的，但计算结果与实验数据存在一定偏差，热力学参数还需要进一步的优化；(c)利用二元系热力学参数外推计算了Sn-Bi-Ni和Bi-Ni-Zn三元系等温截面相图，计算结果与本研究的实验数据吻合的很好；(d)对Ag-Cu-Ni、Ag-Au-Cu、Ag-Au-Ni、Au-Cu-Ni三元系相图进行了热力学计算，计算结果与文献报道的实验数据吻合的比较好。
(3)利用DICTRA软件，根据文献报道的数据对Sn、Ag、Cu、Ni、Au、In、Sb、Zn、Pb等纯组元在其稳定结构中的自扩散系数进行了优化，并采用了文献报道的根据第一原理计算的晶格常数对部分纯组元在Fcc_A1、Bcc_A2、Hcp_A3结构中的自扩散系数进行了计算，初步确定了焊接材料数据库中纯组元的原子移动能力参数；根据文献报道的数据对Sn-Ag-Cu-Au系的各二元系的动力学参数进行了优化，计算结果与实验数据取得了良好的一致性。
(4)举例介绍了无铅焊料热力学数据库在无铅焊料设计、焊料与基板界面反应的预测方面的应用。在本研究中利用热力学计算设计了Bi-Ag-Ni共晶成分的高温无铅焊料，组织观察和熔点测定结果表明计算结果与实验结果取得了良好的一致性。利用热力学数据计算和实验研究了Bi-Ag-Ni焊料与Ni基板的界面反应。同时介绍了无铅焊料动力学数据库在焊料的扩散偶、界面反应时的界面移动方面的应用。
Solders play an important role in the electronic packaging.However,lead (Pb) inthe traditional Sn-Pb based solders is hurtful to the environment and human health.This problem has been paid the attention by all over the world,and many rules werecarried out in USA,Japan,European Unit,and China.Many investigations havefocused on the development of Pb-free solders.According to the recent researches,themost promising candidates should be the multi-component alloys.Thethermodynamic and kinetic calculations have been recognized as an important tool inthe design of materials and investigation on interfacial reaction,because itsignificantly decreases the amount of experimental work.
The purpose of this work is to develop an extensive thermodynamic database anda basic kinetic database.In this work,the phase diagrams in some ternary systemswere determined by EPMA (electron probe micro-analyzer) using equilibrium alloysand diffusion couples,and transformation temperatures of alloys were determined byDSC (differential scanning calorimetry).Based on the experimental data determinedin this work and previous literature,some binary and ternary systems werethermodynamically assessed using the CALPHAD (calculation of phase diagrams)method.The kinetic parameters of pure elements and binary systems were alsooptimized in this work.The details of the results are described as follows:
(1) Based on the experimental method,(a) the isothermal sections at 300℃,400℃,and 500℃of the Sn-Ag-Au system and the transformation temperatures of alloyswere determined;(b) the isothermal sections at 200℃,250℃,300℃,and 400℃ofthe Sn-Au-Bi system and the transformation temperatures of alloys were determined;(c) the isothermal section at 500℃of the Sn-Cu-Ni and Sn-Au-Cu systems weredetermined;(d) the isothermal sections at 300℃,400℃,and 500℃of the Ag-Bi-Niand Cu-Bi-Ni systems were firstly determined;(e) the isothermal sections at 300℃,500℃,and 700℃of the Bi-Ni-Zn system were determined;(f) the phase equilibriainformation on the Sn-Ni and Sn-Bi-Ni systems was determined,which shows that the Ni3Sn4 phase has a large solubility region.A new intermetallic compound ((?)) wasfound in the Sn-Au-Bi system.The space group of the (?) phase is P63/mmc and itscrystal structure is similar with that of the AuSn phase.
(2) Based on the experimental data determined in this work and reported in theprevious literature,(a) the Sn-Ni,Sn-Ag-Au,Sn-Ag-Ni,Sn-Au-Bi,and Cu-Bi-Nisystems were thermodynamically assessed using the CALPHAD method;(b) theSn-Cu-Ni and Sn-Au-Cu systems were basically assessed,where there were slightdeviations between calculated and experimental results,and the thermodynamicparameters should be re-optimized based on further experimental data;(c) theSn-Bi-Ni and Bi-Ni-Zn systems were thermodynamically calculated by extrapolatingthe thermodynamic parameters of the sub-binary systems,and a good agreementbetween calculated and experimental results was obtained;(d) the Ag-Cu-Ni,Ag-Au-Cu,Ag-Au-Ni,and Au-Cu-Ni systems were also thermodynamically assessedas well,and agreement between calculated and experimental results was obtained.
(3) Based on the experimental data,the slef-diffusion coefficients of Sn,Ag,Cu,Ni,Au,In,Sb,Zn,and Pb in their stable structures were optimized in the frame ofDICTRA.The self-diffusion coefficients of the pure elements in the Fcc_A 1,Bcc_A2,and Hcp A3 structures were also calculated.Based on the experimental data,kineticparameters in the sub-binary systems of the Sn-Ag-Cu-Au system were optimized,and a good agreement between calculated and experimental results was obtained.Onthe basis of the kinetic parameters of the pure elements and binary systems,thekinetic database was basically developed.
(4) The present thermodynamic and kinetic databases were applied in the design oflead-free solders,research of interfacial reactions between lead-free solders andsubstrates,and simulation of movement of interface in the soldering process.TheBi-Ag-Ni solder was made on the basis of the calculation in this work.The calculatedresults illustrate that the CALPHAD method is a powerful tool to design lead-freesolders.The kinetic database was applied in the simulation of diffusion couple and themovement of interface in the soldering process.
本研究的主要工作是完善已有的无铅焊料设计系统和初步建立无铅焊料动力学数据库。本研究利用电子探针(EPMA：electron probe micro-analyzer)通过合金法和扩散偶法对部分无铅焊料三元系相平衡进行了实验测定；利用差示扫描量热分析(DSC：differential scanning calorimetry)测定了部分相变温度；利用相图计算的CALPHAD(calculation of phase diagrams)方法对无铅焊料部分二元和三元系的相图进行热力学计算，获得整个体系较为精确的相图和合理的热力学参数，从而完善无铅焊接材料热力学数据库。同时，利用DICTRA软件对纯组元和部分二元系的动力学参数进行优化，初步建立无铅焊接材料动力学数据库。本研究的主要内容如下：
(1)基于合金法和扩散偶法实验方法，(a)测定了Sn-Ag-Au三元系在300℃、400℃和500℃的相平衡和部分不变反应的温度；(b)测定了Sn-Au-Bi三元系在200℃、250℃、300℃和400℃的相平衡和部分不变反应温度，结果表明在Sn-Au-Bi三元系有一个三元金属间化合物(ψ)，该ψ相300℃时固溶度范围为Sn_(12．2)Au_(48．8)Bi_(39)到Sn_(13)Au_(49)Bi_(38)(at．％)，熔点为312．7℃。X-射线衍射分析表明ψ相的空间群为P63／mmc，具有和AuSn相类似的结构；(c)测定了Sn-Cu-Ni和Sn-Au-Cu三元系在500℃的相平衡关系，初步确定了500℃的等温截面相图；(d)测定了Ag-Bi-Ni和Cu-Bi-Ni三元系的相平衡，并首次确定了在300℃、400℃和500℃的Ag-Bi-Ni和Cu-Bi-Ni三元系的等温截面相图，确定了Cu-Bi-Ni三元系300℃在Cu-Ni侧存在一个NiBi+fcc(Cu)+fcc(Ni)的三相平衡区；(e)测定了Bi-Ni-Zn体系在300℃、500℃和700℃的相平衡；(f)测定了Sn-Ni二元系和Sn-Bi-Ni三元系部分相平衡，确定Sn-Ni二元系内不存在NiSn相，而是一个固溶范围较大的Ni_3Sn_4相。
(2)利用CALPHAD方法，根据本研究测定的实验数据和文献报道的实验数据，(a)对Sn-Ni、Sn-Ag-Au、Sn-Ag-Ni、Sn-Au-Bi、Ag-Bi-Ni、Cu-Bi-Ni等体系相图进行了热力学计算，其结果与实验数据吻合的较好：(b)对Sn-Cu-Ni和Sn-Au-Cu三元系相图进行了初步的热力学计算，计算结果与实验数据基本是一致的，但计算结果与实验数据存在一定偏差，热力学参数还需要进一步的优化；(c)利用二元系热力学参数外推计算了Sn-Bi-Ni和Bi-Ni-Zn三元系等温截面相图，计算结果与本研究的实验数据吻合的很好；(d)对Ag-Cu-Ni、Ag-Au-Cu、Ag-Au-Ni、Au-Cu-Ni三元系相图进行了热力学计算，计算结果与文献报道的实验数据吻合的比较好。
(3)利用DICTRA软件，根据文献报道的数据对Sn、Ag、Cu、Ni、Au、In、Sb、Zn、Pb等纯组元在其稳定结构中的自扩散系数进行了优化，并采用了文献报道的根据第一原理计算的晶格常数对部分纯组元在Fcc_A1、Bcc_A2、Hcp_A3结构中的自扩散系数进行了计算，初步确定了焊接材料数据库中纯组元的原子移动能力参数；根据文献报道的数据对Sn-Ag-Cu-Au系的各二元系的动力学参数进行了优化，计算结果与实验数据取得了良好的一致性。
(4)举例介绍了无铅焊料热力学数据库在无铅焊料设计、焊料与基板界面反应的预测方面的应用。在本研究中利用热力学计算设计了Bi-Ag-Ni共晶成分的高温无铅焊料，组织观察和熔点测定结果表明计算结果与实验结果取得了良好的一致性。利用热力学数据计算和实验研究了Bi-Ag-Ni焊料与Ni基板的界面反应。同时介绍了无铅焊料动力学数据库在焊料的扩散偶、界面反应时的界面移动方面的应用。
Solders play an important role in the electronic packaging.However,lead (Pb) inthe traditional Sn-Pb based solders is hurtful to the environment and human health.This problem has been paid the attention by all over the world,and many rules werecarried out in USA,Japan,European Unit,and China.Many investigations havefocused on the development of Pb-free solders.According to the recent researches,themost promising candidates should be the multi-component alloys.Thethermodynamic and kinetic calculations have been recognized as an important tool inthe design of materials and investigation on interfacial reaction,because itsignificantly decreases the amount of experimental work.
The purpose of this work is to develop an extensive thermodynamic database anda basic kinetic database.In this work,the phase diagrams in some ternary systemswere determined by EPMA (electron probe micro-analyzer) using equilibrium alloysand diffusion couples,and transformation temperatures of alloys were determined byDSC (differential scanning calorimetry).Based on the experimental data determinedin this work and previous literature,some binary and ternary systems werethermodynamically assessed using the CALPHAD (calculation of phase diagrams)method.The kinetic parameters of pure elements and binary systems were alsooptimized in this work.The details of the results are described as follows:
(1) Based on the experimental method,(a) the isothermal sections at 300℃,400℃,and 500℃of the Sn-Ag-Au system and the transformation temperatures of alloyswere determined;(b) the isothermal sections at 200℃,250℃,300℃,and 400℃ofthe Sn-Au-Bi system and the transformation temperatures of alloys were determined;(c) the isothermal section at 500℃of the Sn-Cu-Ni and Sn-Au-Cu systems weredetermined;(d) the isothermal sections at 300℃,400℃,and 500℃of the Ag-Bi-Niand Cu-Bi-Ni systems were firstly determined;(e) the isothermal sections at 300℃,500℃,and 700℃of the Bi-Ni-Zn system were determined;(f) the phase equilibriainformation on the Sn-Ni and Sn-Bi-Ni systems was determined,which shows that the Ni3Sn4 phase has a large solubility region.A new intermetallic compound ((?)) wasfound in the Sn-Au-Bi system.The space group of the (?) phase is P63/mmc and itscrystal structure is similar with that of the AuSn phase.
(2) Based on the experimental data determined in this work and reported in theprevious literature,(a) the Sn-Ni,Sn-Ag-Au,Sn-Ag-Ni,Sn-Au-Bi,and Cu-Bi-Nisystems were thermodynamically assessed using the CALPHAD method;(b) theSn-Cu-Ni and Sn-Au-Cu systems were basically assessed,where there were slightdeviations between calculated and experimental results,and the thermodynamicparameters should be re-optimized based on further experimental data;(c) theSn-Bi-Ni and Bi-Ni-Zn systems were thermodynamically calculated by extrapolatingthe thermodynamic parameters of the sub-binary systems,and a good agreementbetween calculated and experimental results was obtained;(d) the Ag-Cu-Ni,Ag-Au-Cu,Ag-Au-Ni,and Au-Cu-Ni systems were also thermodynamically assessedas well,and agreement between calculated and experimental results was obtained.
(3) Based on the experimental data,the slef-diffusion coefficients of Sn,Ag,Cu,Ni,Au,In,Sb,Zn,and Pb in their stable structures were optimized in the frame ofDICTRA.The self-diffusion coefficients of the pure elements in the Fcc_A 1,Bcc_A2,and Hcp A3 structures were also calculated.Based on the experimental data,kineticparameters in the sub-binary systems of the Sn-Ag-Cu-Au system were optimized,and a good agreement between calculated and experimental results was obtained.Onthe basis of the kinetic parameters of the pure elements and binary systems,thekinetic database was basically developed.
(4) The present thermodynamic and kinetic databases were applied in the design oflead-free solders,research of interfacial reactions between lead-free solders andsubstrates,and simulation of movement of interface in the soldering process.TheBi-Ag-Ni solder was made on the basis of the calculation in this work.The calculatedresults illustrate that the CALPHAD method is a powerful tool to design lead-freesolders.The kinetic database was applied in the simulation of diffusion couple and themovement of interface in the soldering process.
引文
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