无铅钎料熔体热力学性质研究及应用
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摘要
无铅锡基钎料是为适应当前环保要求而开发的具有广阔市场应用前景的绿色环保钎料。目前关于无铅钎料合金的研究开发已向多元合金化的方向发展,组元间的相互作用变得更为复杂,单纯用实验的“试凑”的方法难以进行系统化研究,而合金熔体热力学理论是研究合金熔体系统材料组成与相互作用的一门基础科学,是进行材料研究的重要基础理论。由于高温实验的复杂性和精确度的不确定性,通过实验直接测定合金热力学性质受到很大限制,所以目前对三元及多元钎料合金体系的热力学数据实验测定有限,至今仍有大量的热力学数据还未测定,而已开发的无铅钎料合金体系的热力学商用数据库价格昂贵,难以直接进行应用。因此借助合金熔体热力学理论计算来预测钎料合金的热力学性质,从而指导无铅钎料的研究开发,是十分必要和有意义的。
论文主要运用Miedema模型,并结合Chou模型,系统的对主要无铅锡基钎料合金体系熔体热力学参数进行计算、分析及评价,并运用熔体热力学理论对无铅钎料的润湿性、熔化温度、表面张力、界面组织等基础内容进行理论分析。
分别运用Miedema模型和MAEAM模型对主要锡基二元钎料合金体系形成焓进行计算,其中Miedema模型计算值与实测值相差幅度基本在2KJ mol-1以内,具有较好的预测效果,MAEAM模型能够根据具体合金结构进行热力学计算,但预测值明显偏小；而运用Miedema模型与Chou模型相结合的方法对三元锡基钎料合金钎料体系自由能进行计算表明,计算模型具有较高的准确率。
以自由体积理论为基础,运用Miedema模型对二元锡基合金超额熵进行计算,但计算值与实测值存在较大偏差,预测结果无法在较高温度下的热力学计算中应用。
以Miedema模型为基础,对主要的二元及三元无铅钎料合金体系组元的活度及活度系数、活度相互作用系数进行计算,发现活度系数的计算结果基本上能够反映溶质原子和溶剂原子间的相互作用情况,但当组元间相互作用情况过于复杂时,由于Miedema模型本身的局限性,预测值可能会出现较大偏差；而对三元无铅钎料合金体系的活度相互作用系数的计算结果进行理论分析,认为预测模型具有较好的准确性。
通过实验研究了微量元素Pb对Sn-9Zn合金钎料的润湿性的影响,发现Pb可促使Sn-9Zn钎料合金的润湿角下降,润湿面积增大,润湿性得到改善。基于Butler方程,利用Miedema模型结合Chou模型对Sn-Zn、Sn-Pb及Sn-Zn-Pb液态钎料合金体系的表面张力进行计算,模型计算预测值与实测数据在数值大小及变化趋势上均十分相近；同时无论Pb是在全范围内,还是在富Sn端,Pb均使钎料合金表面张力得到下降,从而使Sn-Zn-Pb系三元钎料合金润湿性得到改善。
通过实验研究了微量稀土元素La对Sn3.OAg0.5Cu钎料组织、钎料与Cu基体焊合后界面组织及显微硬度影响,发现La未改变钎料合金的物相构成,但可显著细化钎料组织,钎料/Cu处界面的Cu6Sn5化合物厚度减小,界面形貌变为平坦；同时使Sn3.OAg0.5Cu钎料显微硬度提高14.3%,达到为25HV。通过从活度系数与活度相互作用系数两个方面对Sn-Ag-Cu-La四元合金体系热力学性质进行计算,认为La与Sn、Ag及Cu间强的相互作用趋势,致使钎料组织发生显著细化,同时降低Cu6Sn5/Cu的Cu6Sn5金属间化合物长大驱动力。
通过实验探讨了外加磁场对Sn-9Zn钎料熔化温度的影响,发现0.45T的稳恒静磁场可使Sn-9Zn钎料合金熔化温度下降近2℃,其原因为外加磁场对钎料合金熔体做负功,使原子由液相向固相迁移过程中所需克服的势垒比没有磁场作用时有所增加,致使钎料熔点得到下降。
To meet the requirement of environmental protection, lead-free solder is developed with promising market potential as environment friendly solder. At present, investigation about lead-free solder alloy is tendency of multicomponent alloy, the interaction among components of the solder becomes more complex, experimental "trial and error" approach is difficult to systematically fulfill solder study. On the other hand, alloy molten thermodynamics is fundamental science of component systems, material composition and interaction for alloy molten, which is an important basic theory for material researching and development. Because of the complexity and equipment of experiment being very difficult to guarantee good accuracy under high-temperature, high-temperature experiment is still limited in testing thermodynamics property of alloy molten at present. Therefore, thermodynamic data about ternary and multi-components solder alloy system experimentally determined are limited, and much thermodynamic data has not been determined. On the other hand, business thermodynamic database about lead-free solder alloy is very expensive and it is difficult to apply directly in study. Therefore, with the theoretical calculations, it is very necessary and meaningful to predict thermodynamic properties of molten solder alloy, and to guide the study about lead-free solder as well.
In this paper, using Miedema model, combined with Chou model, molten thermodynamic parameters of major lead-free Tin-based solder alloy system was calculated, analyzed and evaluated. And wettability, melting temperature, surface tension, and interfacial microstructure about lead-free solder was theoretically analyzed from theory of molten thermodynamic as well.
Formation enthalpy for major binary tin-based solder alloy system was calculated, using Miedema model and MAEAM, respectively, in which, difference between predicted value from Miedema model and measured values is less than2KJ mol"1,which indicate that Miedema model, has a good prediction. In spite of relating to specific alloy structure, thermodynamic calculated value from MAEAM model is significantly less than that of measurement. Moreover, free energy for the ternary tin-based solder alloy system was calculated, using Miedema model, combined with Chou model, the calculation model has higher accuracy.
Based on free volume theory, excess entropy of binary Tin-based alloys were calculated, using Miedema model, and found that model has a greater deviation between the calculated values and measured values.Therefore, predicted values can not apple in the thermodynamic calculations about higher temperatures condition.
Based on the Miedema model, activity, activity coefficient and activity interaction coefficients of component for major binary and ternary lead-free solder alloy system were calculated and found that the activity coefficient from calculations can basically reflect the interaction between solute atoms and solvent atoms. When element interaction among the components of the solder, is too complicated, due to the limitations of Miedema model itself, predictive value could be greater of the deviation, however, based on calculating and theoretical analysis about activity interaction coefficient of the ternary lead-free solder alloy system, the prediction model has good precision.
Effect of trace elements Pb on wettability of Sn-9Zn solder was investigated through experiments, and found that Pb can decrease wetting angle of Sn-9Zn solder alloy, and increase wetting area, which improve wettability of Sn-9Zn solder. Based on Butler equation, surface tension liquid solder of Sn-Zn, Sn-Pb and Sn-Zn-Pb solder alloy systems was calculated using Miedema model with Chou model, values calculated the model is very similar to measured values not only in the magnitude aspect but also trend in aspect. Based on the calculating from whole range of Pb and Sn-rich side in the Sn-Zn solder, Pb can decline surface tension of the solder, which improve wettability of Sn-Zn-Pb solder ternary alloy system.
Effect of trace rare earth elements La on microstructure, interfacial microstructure between the solder and Cu substrate and microhardness for Sn3.OAgO.5Cu solder was investigated through experiments, and found that La do not change component phase of the solder, however, microstructure of the solder significantly fine and thickness of Cu6Sn5compounds the solder/Cu at the interface decrease, the interface morphology becomes flat at the same time. Moreover, microhardness of Sn3.OAgO.5Cu solder increased14.3%, reaching to25HV. From the component activity coefficient and activity interaction coefficient, thermodynamic properties of Sn-Ag-Cu-La quaternary alloy system was calculated and find that strong interaction trend between La and the component of Sn, Ag and Cu respectively, can significant fine microstructure of the solder, and reduce the growth driving force of intermetallic compounds for Cu6Sn5of Cu6Sn5/Cu interface at same time.
Effect of the external magnetic field on melting temperature for Sn-9Zn solder was investigated through experiments, and found that0.45T static steady magnetic field can drop melting temperature of Sn-9Zn solder alloy to nearly2℃.Comparing to no magnetic field to the solder, the potential barrier overcome by the atoms migration from the liquid phase to the solid phase is increase, which lead to the solder melting point drop.
论文主要运用Miedema模型,并结合Chou模型,系统的对主要无铅锡基钎料合金体系熔体热力学参数进行计算、分析及评价,并运用熔体热力学理论对无铅钎料的润湿性、熔化温度、表面张力、界面组织等基础内容进行理论分析。
分别运用Miedema模型和MAEAM模型对主要锡基二元钎料合金体系形成焓进行计算,其中Miedema模型计算值与实测值相差幅度基本在2KJ mol-1以内,具有较好的预测效果,MAEAM模型能够根据具体合金结构进行热力学计算,但预测值明显偏小；而运用Miedema模型与Chou模型相结合的方法对三元锡基钎料合金钎料体系自由能进行计算表明,计算模型具有较高的准确率。
以自由体积理论为基础,运用Miedema模型对二元锡基合金超额熵进行计算,但计算值与实测值存在较大偏差,预测结果无法在较高温度下的热力学计算中应用。
以Miedema模型为基础,对主要的二元及三元无铅钎料合金体系组元的活度及活度系数、活度相互作用系数进行计算,发现活度系数的计算结果基本上能够反映溶质原子和溶剂原子间的相互作用情况,但当组元间相互作用情况过于复杂时,由于Miedema模型本身的局限性,预测值可能会出现较大偏差；而对三元无铅钎料合金体系的活度相互作用系数的计算结果进行理论分析,认为预测模型具有较好的准确性。
通过实验研究了微量元素Pb对Sn-9Zn合金钎料的润湿性的影响,发现Pb可促使Sn-9Zn钎料合金的润湿角下降,润湿面积增大,润湿性得到改善。基于Butler方程,利用Miedema模型结合Chou模型对Sn-Zn、Sn-Pb及Sn-Zn-Pb液态钎料合金体系的表面张力进行计算,模型计算预测值与实测数据在数值大小及变化趋势上均十分相近；同时无论Pb是在全范围内,还是在富Sn端,Pb均使钎料合金表面张力得到下降,从而使Sn-Zn-Pb系三元钎料合金润湿性得到改善。
通过实验研究了微量稀土元素La对Sn3.OAg0.5Cu钎料组织、钎料与Cu基体焊合后界面组织及显微硬度影响,发现La未改变钎料合金的物相构成,但可显著细化钎料组织,钎料/Cu处界面的Cu6Sn5化合物厚度减小,界面形貌变为平坦；同时使Sn3.OAg0.5Cu钎料显微硬度提高14.3%,达到为25HV。通过从活度系数与活度相互作用系数两个方面对Sn-Ag-Cu-La四元合金体系热力学性质进行计算,认为La与Sn、Ag及Cu间强的相互作用趋势,致使钎料组织发生显著细化,同时降低Cu6Sn5/Cu的Cu6Sn5金属间化合物长大驱动力。
通过实验探讨了外加磁场对Sn-9Zn钎料熔化温度的影响,发现0.45T的稳恒静磁场可使Sn-9Zn钎料合金熔化温度下降近2℃,其原因为外加磁场对钎料合金熔体做负功,使原子由液相向固相迁移过程中所需克服的势垒比没有磁场作用时有所增加,致使钎料熔点得到下降。
To meet the requirement of environmental protection, lead-free solder is developed with promising market potential as environment friendly solder. At present, investigation about lead-free solder alloy is tendency of multicomponent alloy, the interaction among components of the solder becomes more complex, experimental "trial and error" approach is difficult to systematically fulfill solder study. On the other hand, alloy molten thermodynamics is fundamental science of component systems, material composition and interaction for alloy molten, which is an important basic theory for material researching and development. Because of the complexity and equipment of experiment being very difficult to guarantee good accuracy under high-temperature, high-temperature experiment is still limited in testing thermodynamics property of alloy molten at present. Therefore, thermodynamic data about ternary and multi-components solder alloy system experimentally determined are limited, and much thermodynamic data has not been determined. On the other hand, business thermodynamic database about lead-free solder alloy is very expensive and it is difficult to apply directly in study. Therefore, with the theoretical calculations, it is very necessary and meaningful to predict thermodynamic properties of molten solder alloy, and to guide the study about lead-free solder as well.
In this paper, using Miedema model, combined with Chou model, molten thermodynamic parameters of major lead-free Tin-based solder alloy system was calculated, analyzed and evaluated. And wettability, melting temperature, surface tension, and interfacial microstructure about lead-free solder was theoretically analyzed from theory of molten thermodynamic as well.
Formation enthalpy for major binary tin-based solder alloy system was calculated, using Miedema model and MAEAM, respectively, in which, difference between predicted value from Miedema model and measured values is less than2KJ mol"1,which indicate that Miedema model, has a good prediction. In spite of relating to specific alloy structure, thermodynamic calculated value from MAEAM model is significantly less than that of measurement. Moreover, free energy for the ternary tin-based solder alloy system was calculated, using Miedema model, combined with Chou model, the calculation model has higher accuracy.
Based on free volume theory, excess entropy of binary Tin-based alloys were calculated, using Miedema model, and found that model has a greater deviation between the calculated values and measured values.Therefore, predicted values can not apple in the thermodynamic calculations about higher temperatures condition.
Based on the Miedema model, activity, activity coefficient and activity interaction coefficients of component for major binary and ternary lead-free solder alloy system were calculated and found that the activity coefficient from calculations can basically reflect the interaction between solute atoms and solvent atoms. When element interaction among the components of the solder, is too complicated, due to the limitations of Miedema model itself, predictive value could be greater of the deviation, however, based on calculating and theoretical analysis about activity interaction coefficient of the ternary lead-free solder alloy system, the prediction model has good precision.
Effect of trace elements Pb on wettability of Sn-9Zn solder was investigated through experiments, and found that Pb can decrease wetting angle of Sn-9Zn solder alloy, and increase wetting area, which improve wettability of Sn-9Zn solder. Based on Butler equation, surface tension liquid solder of Sn-Zn, Sn-Pb and Sn-Zn-Pb solder alloy systems was calculated using Miedema model with Chou model, values calculated the model is very similar to measured values not only in the magnitude aspect but also trend in aspect. Based on the calculating from whole range of Pb and Sn-rich side in the Sn-Zn solder, Pb can decline surface tension of the solder, which improve wettability of Sn-Zn-Pb solder ternary alloy system.
Effect of trace rare earth elements La on microstructure, interfacial microstructure between the solder and Cu substrate and microhardness for Sn3.OAgO.5Cu solder was investigated through experiments, and found that La do not change component phase of the solder, however, microstructure of the solder significantly fine and thickness of Cu6Sn5compounds the solder/Cu at the interface decrease, the interface morphology becomes flat at the same time. Moreover, microhardness of Sn3.OAgO.5Cu solder increased14.3%, reaching to25HV. From the component activity coefficient and activity interaction coefficient, thermodynamic properties of Sn-Ag-Cu-La quaternary alloy system was calculated and find that strong interaction trend between La and the component of Sn, Ag and Cu respectively, can significant fine microstructure of the solder, and reduce the growth driving force of intermetallic compounds for Cu6Sn5of Cu6Sn5/Cu interface at same time.
Effect of the external magnetic field on melting temperature for Sn-9Zn solder was investigated through experiments, and found that0.45T static steady magnetic field can drop melting temperature of Sn-9Zn solder alloy to nearly2℃.Comparing to no magnetic field to the solder, the potential barrier overcome by the atoms migration from the liquid phase to the solid phase is increase, which lead to the solder melting point drop.
引文
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