焊料纳米改性对无铅焊点界面反应及力学性能影响的研究
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摘要
微电子产品的无铅化、小型化的趋势使得互连界面的脆性金属间化合物（IMC）趋向于占据更大的焊点体积份额，甚至使得互连焊点界面只包含几个IMC晶粒，成为影响微电子产品可靠性的关键科学问题。针对微电子封装可靠性的关键性问题，论文系统地研究了回流焊和时效过程中掺杂TiO_2纳米颗粒对IMC生长、互连界面微观结构和力学性能的影响机理，探索了有效抑制IMC生长和改善互连可靠性的掺杂方案，研究了无铅纳米复合焊料与焊盘金属基体（Cu基板）间界面反应动力学、焊点界面微观结构在时效过程中的演变对焊点可靠性的影响机理和应变速率及温度对复合焊料合金力学性能的影响，优化了无铅纳米复合焊料，为增强无铅焊接的可靠性提供设计、工艺和材料等方面的参考数据。其研究的主要结果如下：
研究TiO_2纳米颗粒掺杂对Sn-3.0Ag-0.5Cu-xTiO_2(x=0,0.02,0.05,0.1,0.3和0.6wt.%)复合焊料的熔点、润湿性及显微组织影响的结果表明，掺杂TiO_2纳米颗粒对复合焊料熔点影响不大，但其与Cu基板的润湿性稍有提高。当TiO_2纳米颗粒的含量为0.1wt.%时，复合焊料与Cu基板的润湿性最好，其表面接触角最小值为8.4o，铺展面积最大值为155.24mm~2。电子扫描显微镜照片显示掺杂明显地细化了焊料基体的显微组织，其可能的机理为TiO_2纳米颗粒的表面吸附效应降低了复合焊料基体组织中Ag_3Sn晶粒的表面能，抑制了Ag_3Sn晶粒的生长和异常长大，从而细化了复合焊料的显微组织。
研究TiO_2纳米颗粒掺杂对焊点在回流焊过程中界面液-固反应影响的结果表明，一部分TiO_2纳米颗粒会溶解在富Sn相中，一部分TiO_2纳米颗粒会沉降在Ag_3Sn相表面，还有一部分TiO_2纳米颗粒会沉降在Cu_6Sn_5相表面。掺杂TiO_2纳米颗粒后焊点界面IMC层厚度和IMC晶粒尺寸均减少。研究IMC生长指数结果表明，界面润湿反应的IMC生长是一种混合生长机制，IMC生长过程可分为三个阶段：包括扩散反应阶段、元素经晶粒间扩散的IMC扩散控制生长阶段和元素经IMC层扩散的IMC控制生长阶段。对IMC晶粒生长指数的研究结果表明，IMC晶粒生长是由原子互扩散和晶粒成熟共同控制。当TiO_2纳米颗粒含量为0.1wt.%时，IMC生长速率有最小值，抑制界面IMC层生长和细化IMC晶粒效果最显著。为了更好地理解界面反应和IMC生长机理，基于固体扩散理论建立了双相位滞后扩散模型和波动模型，模拟了回流焊过程中IMC层生长动力学；建立了Cu原子扩散通量驱动晶粒成熟生长模型，分析了回流焊过程中IMC晶粒生长机理。结果表明，回流焊过程中TiO_2纳米颗粒影响IMC生长机理符合异相成核和奥斯瓦尔德晶粒成熟机制。
研究TiO_2纳米颗粒掺杂对焊点在120℃，150℃和190℃时效条件下界面固-固反应影响的结果表明，掺杂TiO_2纳米颗粒后焊点界面IMC层厚度减小，当TiO_2纳米颗粒含量为0.05-0.1wt.%时，IMC层厚度下降最显著。将Cu_6Sn_5和Cu_3Sn相看成一个整体时，界面IMC生长受扩散定律控制。将Cu_6Sn_5和Cu_3Sn相分别看成一个独立实体时，在190℃高温时效条件下，IMC层的生长主要是由扩散机制控制，而在120℃低温时效条件下，IMC层的生长是由扩散和界面反应共同控制。掺杂TiO_2纳米颗粒可以提高Cu_6Sn_5和Cu_3Sn相IMC层的活化能，减少原子的互扩散速率，从而抑制界面IMC层生长。比较Cu_6Sn_5和Cu_3Sn相IMC层的活化能可知，Cu_3Sn相IMC层有更高的活化能。观察焊点的微观结构演变可知，时效过程中掺杂TiO_2纳米颗粒抑制IMC生长机理可能为晶界钉扎机制。
研究TiO_2纳米颗粒掺杂对Sn-3.0Ag-0.5Cu-xTiO_2复合焊料合金及焊点力学性能影响的结果表明，掺杂TiO_2纳米颗粒后复合焊料合金的显微硬度提高19%-37%。这种明显的强化效果是由于掺杂TiO_2纳米颗粒后减小了Ag_3Sn晶粒的平均尺寸和间距。复合焊料合金的极限拉伸强度（UTS）随着应变速率对数的增加而线性增大，随着温度的升高而线性减小。这是由于应变速率增加后位错增多，导致位错密度增加，位错间相互作用增强，从而提高复合焊料合金的抗形变能力。复合焊料焊点的拉伸强度随着时效时间的增加而减小。随着时效时间的增加，界面IMC层的生长导致焊点断裂模式发生变化，由最初的在焊料内部的韧性断裂变为既有韧性断裂又有脆性断裂的混合断裂模式，到最后沿着界面IMC的脆性断裂。研究结果还表明，含TiO_2纳米颗粒的复合焊料合金和焊点的拉伸强度比不含TiO_2纳米颗粒的焊料大，其机理可能为固溶强化和颗粒硬化机制。
With the trend towards miniaturization of microelectronic products andimplementation of lead-free soldering, the size of the microelectronic components and thusthe solder joints has been scaled down. As a result, the percentage of the volume of thebrittle intermetallic compounds (IMC) layer in solder joints trends to become higher, andpossibly only a few IMC grains is interconnected with solder joint interface, resulting inmore brittle fracture and affect the reliability of microelectronic products. Focusing on thekey issues of the reliability of microelectronic packaging, the influence of TiO_2nanoparticles dopant on the IMC growth, interconnection interface microstructure, andmechanical properties in reflow and aging processes has been investigated. The mechanismof effective inhibition of IMC growth and the doping scheme for the improvement of theinterconnect reliability have been explored. The interface reaction kinetics betweenlead-free nano-composite solder and Cu substrate, the effect of interface microstructureevolution on the reliability of solder joints during aging process, and the effect of strainrate and temperature on the mechanical properties of composite solder alloys have beensystematically investigated. The nano-composite solder has been optimized. The resultsachieved in the thesis can provide the reference in aspects of the solder joint reliabilitydesign, process and materials. The main conclusions obtained are as follows:
The influence of TiO_2nanoparticles dopant on the melting point, wettability andmicrostructure in Sn-3.0Ag-0.5Cu-xTiO_2(x=0,0.02,0.05,0.1,0.3, and0.6wt.%)composite solders have been investigated. Results show that the melting points of theTiO_2-containing composite solders have no obvious change compared with TiO_2-freesolders. However, with an increase in the proportion of TiO_2nanoparticles, the wettabilityof the composite solders slightly increase and the microstructure of composite soldermatrix has obviously been changed. When the weight percentage of TiO_2nanoparticles is0.1wt.%, the wettability of composite solder is the best, the surface contact angle has aminimum value of8.40, while the spreading area has a maximum value of155.24mm~2.SEM photos show that dopant significantly refine the microstructure of the solder matrix. This is because the adsorption effect on the surface of TiO_2nanoparticles can reduce thesurface energy of Ag_3Sn grains in the composite solder matrix and inhibit the Ag_3Sn grainsgrowth.
The influence of TiO_2nanoparticles dopant on liquid-solid interface reaction inSn-3.0Ag-0.5Cu-xTiO_2solder joints in reflow process has been investigated. Results showthat some of TiO_2nanoparticles are dissolved in the Sn-rich phase, some of themparticipate in the surface of Ag_3Sn phase, and the rest dissolves in surface of the Cu_6Sn_5IMC layer. Both of the thickness and grain size of IMC decrease when TiO_2nanoparticlesis added into the Sn-3.0Ag-0.5Cu solder system. According to the results of the IMC layergrowth exponents, it can be found that the growth kinetics of interfacical IMC layer is amixed growth mechanism. The wetting reaction process may contain three stages: thereaction diffusion stage, the grain boundary diffusion controlled IMC growth stage, and thevolume diffusion controlled IMC growth stage. The results of the IMC grain exponentsshow that the growth of IMC grains is controlled by atomic interdiffusion and grainmaturity. The data also show that Sn-3.0Ag-0.5Cu with about0.1wt.%TiO_2nanoparticlessolder system exhibits the smallest growth rate and gives the most prominent effect inretarding IMC growth and refining IMC grain size. In order to better understand theinterface reaction and IMC growth mechanism, a dual phase lag diffusion model and awave model based on the solid-state diffusion theory are presented for predicting the IMClayer growth in reflow process. A flux-driven ripening of copper-tin scallops is presentedfor predicting the IMC grain growth in reflow process. Based on the observation of themicrostructural evolution of the solder joints, a heterogeneous nucleation mechanism andOstwald grain ripening mechanism for retarding the IMC layer growth and refining theIMC grains due to TiO_2nanoparticles addition is proposed.
The influence of TiO_2nanoparticles dopant on solid-solid interface reaction inSn-3.0Ag-0.5Cu-xTiO_2solder joints in120℃,150℃, and190℃aging process have beeninvestigated. Results show that the thickness of IMC decreases when TiO_2nanoparticlesare added into Sn-3.0Ag-0.5Cu solder system. There is a significant drop in IMC thickness when the weight percentage of TiO_2nanoparticles reaches0.05-0.1wt.%. When takenCu_6Sn_5and Cu_3Sn as a single entity, the IMC layer growth may be mainly controlled by aninterdiffusion-controlled mechanism. When taken Cu_6Sn_5and Cu_3Sn as independententities, at190℃higher aging temperature, the growth for both the Cu_6Sn_5and Cu_3SnIMC layers might be controlled by diffusion. At120℃lower aging temperature, thegrowth for both the Cu_6Sn_5and Cu_3Sn IMC layers are not compoletely diffusion controlled,bus also affected by chemical reaction. Results also show that adding TiO_2nanoparticles inSn-3.0Ag-0.5Cu solder system can increase the activation energy, and thus reduce theatomic diffusion rate, so as to inhibit the excessive growth of the IMC. Compared withCu_6Sn_5IMC layer, Cu_3Sn IMC layer has much higher activation energy. Based on theobservation of the microstructural evolution of the solder joints, a grain boundary pinningmechanism for inhibition of the IMC growth in aging process due to TiO_2nanoparticles isproposed.
The influence of TiO_2nanoparticles dopant on mechanical properties inSn-3.0Ag-0.5Cu-xTiO_2composite solder alloys and solder joints have been investigated.Results show that the microhardness enhancement of these TiO_2-containing compositesolders is19%to37%compared with TiO_2-free noncomposite solder. The existence ofTiO_2nanoparticles in the solder matrix can apparently enhance the microhardness of thecomposite solder. This might be attributed to the reduction of the size and spacing betweenAg_3Sn grains in the solder matrix. The ultimate tensile strength (UTS) ofSn-3.0Ag-0.5Cu-xTiO_2composite solder alloys has a logarithmically linear increaserelation with strain rate and has a linear decrease with temperature. At higher strain rate,more and more dislocations are created. Increasing strain rate is accompanied by anincrease in the dislocation density. The increase in dislocation density will in turn increasethe interaction between dislocations and result in improving the composite solder alloysresistance to deformation. Tensile strength of solder joints drops with the aging time. Withan increase in aging time, the growth of interfacial IMC layer leads to change the fracturepattern in solder joints. The fracture pattern can be classified into three types with the increase in ageing time: ductile fracture in the solder at the begining, and then mixedfracture type containing ductile fracture and brittle fracture, and lately the brittle fracturealong the IMC interface for the long aging time. TiO_2-containing composite solder alloysand solder joints have higher UTS than TiO_2-free solder alloy and solder joint due to solidhardening and paricle hardening.
研究TiO_2纳米颗粒掺杂对Sn-3.0Ag-0.5Cu-xTiO_2(x=0,0.02,0.05,0.1,0.3和0.6wt.%)复合焊料的熔点、润湿性及显微组织影响的结果表明，掺杂TiO_2纳米颗粒对复合焊料熔点影响不大，但其与Cu基板的润湿性稍有提高。当TiO_2纳米颗粒的含量为0.1wt.%时，复合焊料与Cu基板的润湿性最好，其表面接触角最小值为8.4o，铺展面积最大值为155.24mm~2。电子扫描显微镜照片显示掺杂明显地细化了焊料基体的显微组织，其可能的机理为TiO_2纳米颗粒的表面吸附效应降低了复合焊料基体组织中Ag_3Sn晶粒的表面能，抑制了Ag_3Sn晶粒的生长和异常长大，从而细化了复合焊料的显微组织。
研究TiO_2纳米颗粒掺杂对焊点在回流焊过程中界面液-固反应影响的结果表明，一部分TiO_2纳米颗粒会溶解在富Sn相中，一部分TiO_2纳米颗粒会沉降在Ag_3Sn相表面，还有一部分TiO_2纳米颗粒会沉降在Cu_6Sn_5相表面。掺杂TiO_2纳米颗粒后焊点界面IMC层厚度和IMC晶粒尺寸均减少。研究IMC生长指数结果表明，界面润湿反应的IMC生长是一种混合生长机制，IMC生长过程可分为三个阶段：包括扩散反应阶段、元素经晶粒间扩散的IMC扩散控制生长阶段和元素经IMC层扩散的IMC控制生长阶段。对IMC晶粒生长指数的研究结果表明，IMC晶粒生长是由原子互扩散和晶粒成熟共同控制。当TiO_2纳米颗粒含量为0.1wt.%时，IMC生长速率有最小值，抑制界面IMC层生长和细化IMC晶粒效果最显著。为了更好地理解界面反应和IMC生长机理，基于固体扩散理论建立了双相位滞后扩散模型和波动模型，模拟了回流焊过程中IMC层生长动力学；建立了Cu原子扩散通量驱动晶粒成熟生长模型，分析了回流焊过程中IMC晶粒生长机理。结果表明，回流焊过程中TiO_2纳米颗粒影响IMC生长机理符合异相成核和奥斯瓦尔德晶粒成熟机制。
研究TiO_2纳米颗粒掺杂对焊点在120℃，150℃和190℃时效条件下界面固-固反应影响的结果表明，掺杂TiO_2纳米颗粒后焊点界面IMC层厚度减小，当TiO_2纳米颗粒含量为0.05-0.1wt.%时，IMC层厚度下降最显著。将Cu_6Sn_5和Cu_3Sn相看成一个整体时，界面IMC生长受扩散定律控制。将Cu_6Sn_5和Cu_3Sn相分别看成一个独立实体时，在190℃高温时效条件下，IMC层的生长主要是由扩散机制控制，而在120℃低温时效条件下，IMC层的生长是由扩散和界面反应共同控制。掺杂TiO_2纳米颗粒可以提高Cu_6Sn_5和Cu_3Sn相IMC层的活化能，减少原子的互扩散速率，从而抑制界面IMC层生长。比较Cu_6Sn_5和Cu_3Sn相IMC层的活化能可知，Cu_3Sn相IMC层有更高的活化能。观察焊点的微观结构演变可知，时效过程中掺杂TiO_2纳米颗粒抑制IMC生长机理可能为晶界钉扎机制。
研究TiO_2纳米颗粒掺杂对Sn-3.0Ag-0.5Cu-xTiO_2复合焊料合金及焊点力学性能影响的结果表明，掺杂TiO_2纳米颗粒后复合焊料合金的显微硬度提高19%-37%。这种明显的强化效果是由于掺杂TiO_2纳米颗粒后减小了Ag_3Sn晶粒的平均尺寸和间距。复合焊料合金的极限拉伸强度（UTS）随着应变速率对数的增加而线性增大，随着温度的升高而线性减小。这是由于应变速率增加后位错增多，导致位错密度增加，位错间相互作用增强，从而提高复合焊料合金的抗形变能力。复合焊料焊点的拉伸强度随着时效时间的增加而减小。随着时效时间的增加，界面IMC层的生长导致焊点断裂模式发生变化，由最初的在焊料内部的韧性断裂变为既有韧性断裂又有脆性断裂的混合断裂模式，到最后沿着界面IMC的脆性断裂。研究结果还表明，含TiO_2纳米颗粒的复合焊料合金和焊点的拉伸强度比不含TiO_2纳米颗粒的焊料大，其机理可能为固溶强化和颗粒硬化机制。
With the trend towards miniaturization of microelectronic products andimplementation of lead-free soldering, the size of the microelectronic components and thusthe solder joints has been scaled down. As a result, the percentage of the volume of thebrittle intermetallic compounds (IMC) layer in solder joints trends to become higher, andpossibly only a few IMC grains is interconnected with solder joint interface, resulting inmore brittle fracture and affect the reliability of microelectronic products. Focusing on thekey issues of the reliability of microelectronic packaging, the influence of TiO_2nanoparticles dopant on the IMC growth, interconnection interface microstructure, andmechanical properties in reflow and aging processes has been investigated. The mechanismof effective inhibition of IMC growth and the doping scheme for the improvement of theinterconnect reliability have been explored. The interface reaction kinetics betweenlead-free nano-composite solder and Cu substrate, the effect of interface microstructureevolution on the reliability of solder joints during aging process, and the effect of strainrate and temperature on the mechanical properties of composite solder alloys have beensystematically investigated. The nano-composite solder has been optimized. The resultsachieved in the thesis can provide the reference in aspects of the solder joint reliabilitydesign, process and materials. The main conclusions obtained are as follows:
The influence of TiO_2nanoparticles dopant on the melting point, wettability andmicrostructure in Sn-3.0Ag-0.5Cu-xTiO_2(x=0,0.02,0.05,0.1,0.3, and0.6wt.%)composite solders have been investigated. Results show that the melting points of theTiO_2-containing composite solders have no obvious change compared with TiO_2-freesolders. However, with an increase in the proportion of TiO_2nanoparticles, the wettabilityof the composite solders slightly increase and the microstructure of composite soldermatrix has obviously been changed. When the weight percentage of TiO_2nanoparticles is0.1wt.%, the wettability of composite solder is the best, the surface contact angle has aminimum value of8.40, while the spreading area has a maximum value of155.24mm~2.SEM photos show that dopant significantly refine the microstructure of the solder matrix. This is because the adsorption effect on the surface of TiO_2nanoparticles can reduce thesurface energy of Ag_3Sn grains in the composite solder matrix and inhibit the Ag_3Sn grainsgrowth.
The influence of TiO_2nanoparticles dopant on liquid-solid interface reaction inSn-3.0Ag-0.5Cu-xTiO_2solder joints in reflow process has been investigated. Results showthat some of TiO_2nanoparticles are dissolved in the Sn-rich phase, some of themparticipate in the surface of Ag_3Sn phase, and the rest dissolves in surface of the Cu_6Sn_5IMC layer. Both of the thickness and grain size of IMC decrease when TiO_2nanoparticlesis added into the Sn-3.0Ag-0.5Cu solder system. According to the results of the IMC layergrowth exponents, it can be found that the growth kinetics of interfacical IMC layer is amixed growth mechanism. The wetting reaction process may contain three stages: thereaction diffusion stage, the grain boundary diffusion controlled IMC growth stage, and thevolume diffusion controlled IMC growth stage. The results of the IMC grain exponentsshow that the growth of IMC grains is controlled by atomic interdiffusion and grainmaturity. The data also show that Sn-3.0Ag-0.5Cu with about0.1wt.%TiO_2nanoparticlessolder system exhibits the smallest growth rate and gives the most prominent effect inretarding IMC growth and refining IMC grain size. In order to better understand theinterface reaction and IMC growth mechanism, a dual phase lag diffusion model and awave model based on the solid-state diffusion theory are presented for predicting the IMClayer growth in reflow process. A flux-driven ripening of copper-tin scallops is presentedfor predicting the IMC grain growth in reflow process. Based on the observation of themicrostructural evolution of the solder joints, a heterogeneous nucleation mechanism andOstwald grain ripening mechanism for retarding the IMC layer growth and refining theIMC grains due to TiO_2nanoparticles addition is proposed.
The influence of TiO_2nanoparticles dopant on solid-solid interface reaction inSn-3.0Ag-0.5Cu-xTiO_2solder joints in120℃,150℃, and190℃aging process have beeninvestigated. Results show that the thickness of IMC decreases when TiO_2nanoparticlesare added into Sn-3.0Ag-0.5Cu solder system. There is a significant drop in IMC thickness when the weight percentage of TiO_2nanoparticles reaches0.05-0.1wt.%. When takenCu_6Sn_5and Cu_3Sn as a single entity, the IMC layer growth may be mainly controlled by aninterdiffusion-controlled mechanism. When taken Cu_6Sn_5and Cu_3Sn as independententities, at190℃higher aging temperature, the growth for both the Cu_6Sn_5and Cu_3SnIMC layers might be controlled by diffusion. At120℃lower aging temperature, thegrowth for both the Cu_6Sn_5and Cu_3Sn IMC layers are not compoletely diffusion controlled,bus also affected by chemical reaction. Results also show that adding TiO_2nanoparticles inSn-3.0Ag-0.5Cu solder system can increase the activation energy, and thus reduce theatomic diffusion rate, so as to inhibit the excessive growth of the IMC. Compared withCu_6Sn_5IMC layer, Cu_3Sn IMC layer has much higher activation energy. Based on theobservation of the microstructural evolution of the solder joints, a grain boundary pinningmechanism for inhibition of the IMC growth in aging process due to TiO_2nanoparticles isproposed.
The influence of TiO_2nanoparticles dopant on mechanical properties inSn-3.0Ag-0.5Cu-xTiO_2composite solder alloys and solder joints have been investigated.Results show that the microhardness enhancement of these TiO_2-containing compositesolders is19%to37%compared with TiO_2-free noncomposite solder. The existence ofTiO_2nanoparticles in the solder matrix can apparently enhance the microhardness of thecomposite solder. This might be attributed to the reduction of the size and spacing betweenAg_3Sn grains in the solder matrix. The ultimate tensile strength (UTS) ofSn-3.0Ag-0.5Cu-xTiO_2composite solder alloys has a logarithmically linear increaserelation with strain rate and has a linear decrease with temperature. At higher strain rate,more and more dislocations are created. Increasing strain rate is accompanied by anincrease in the dislocation density. The increase in dislocation density will in turn increasethe interaction between dislocations and result in improving the composite solder alloysresistance to deformation. Tensile strength of solder joints drops with the aging time. Withan increase in aging time, the growth of interfacial IMC layer leads to change the fracturepattern in solder joints. The fracture pattern can be classified into three types with the increase in ageing time: ductile fracture in the solder at the begining, and then mixedfracture type containing ductile fracture and brittle fracture, and lately the brittle fracturealong the IMC interface for the long aging time. TiO_2-containing composite solder alloysand solder joints have higher UTS than TiO_2-free solder alloy and solder joint due to solidhardening and paricle hardening.
引文
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