快速凝固及微合金化Sn-Zn系钎料改性研究
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摘要
Pb及其化合物由于对人类健康和环境具有毒害作用而被禁用。随着无铅化进程的日益深入，无铅钎料的开发和应用已经成为电子封装工业中的关键技术。Sn-Zn系合金熔点与材料成本低且具有优良的力学性能，被认为是能够替代传统Sn-Pb合金用于电子封装与互联的无铅钎料合金系之一。但是，由于Zn非常活泼，Sn-Zn系合金的润湿性、耐蚀与抗高温氧化性能较差且焊点具有脆化倾向。
针对Sn-Zn系钎料合金所存在的问题，本文以共晶Sn-Zn无铅钎料作为参照物，研究了快速凝固及微合金化对Sn-Zn系钎料显微结构、合金特性、钎料/Cu界面行为及焊点力学性能的影响。
研究表明，Sn-Zn钎料/Cu焊点界面紧靠Cu基板侧形成CuZn金属间化合物（IMC）层，CuZn IMC有与钎料中的Zn原子继续反应生成Cu_5Zn_8的趋势；Cu原子越过Sn-Zn钎料/Cu基板界面IMC层向钎料中的扩散与聚集呈现“脉动”形式，并在邻近结合面的钎料中形成粒状Cu_5Zn_8IMC；Sn-Zn钎料与Cu基板界面IMC主要表现为3种形貌：粗糙的界面Cu_5Zn_8IMC层、致密的Cu_5Zn_8胞状晶层、板状CuZn IMC层。
合金微观分析表明，Sn-Zn钎料在本试验快速凝固条件下，初生β-Sn相快速生长与分枝形成网络状枝晶，Zn相的长大被抑制，呈尺寸为0.5~2μm的细小颗粒状被包覆于β-Sn枝晶中；与Sn-9Zn合金相比，0.1wt.%Cr的添加对基体组织的细化作用促进了快速凝固过程中Zn在Sn中的固溶，组织中β-Sn相枝晶更为均匀，颗粒状Zn相更为细小（尺寸基本上不大于1μm）且分布更为弥散；快速凝固态Sn-8Zn-3Bi合金中，Zn相以不规则的尺寸大致为2-4μm的细小条块状或颗粒状分布于Sn枝晶中，Bi均以过饱和固溶体形式存在于Sn相中。
钎料熔化特性分析结果表明，经本文工艺条件下快速凝固制备后，Sn-Zn合金的熔点几乎无变化，Sn-9Zn-0.1Cr合金的熔点降低约9°C，而Sn-8Zn-3Bi合金由于Bi完全固溶在Sn中导致熔点反而升高了约7°C；与常态合金相比，处于热力学亚稳定状态的快速凝固态Sn-Zn系合金熔化区间均显著减小，在钎焊加热过程中结晶潜热的释放促进了钎料对基板的润湿与铺展。
Sn-Zn/Cu界面IMC分析表明，快速凝固态钎料中细小的Zn相与析出相在钎焊过程中与基板元素间的反应均匀，避免了界面处粗大块状Cu_5Zn_8IMC的形成，能够促进钎焊时均匀界面反应层的形成，显著提高了焊点结合强度。
150°C长时间时效会导致Sn-Zn/Cu焊点界面Cu-Zn化合物的分解，IMC层厚度表现为随时间的延长先增大而后减小的趋势，局部被破坏的界面区Cu基体处形成Cu_6Sn_5化合物；与常态钎料相比，使用快速凝固态Sn-Zn钎料所形成的较为均匀致密的界面IMC层在高温时效过程中较稳定。
界面IMC生长动力学分析结果表明：适量合金元素Cr、Bi在Sn-9Zn合金中的添加能够抑制钎焊过程中界面Cu-Zn IMC的生长；本文试验条件下，钎焊温度为240°C时钎料/Cu基板钎焊过程中IMC生长速率常数k分别为：使用Sn-9Zn钎料时约为3.5，使用Sn-9Zn-0.1Cr或Sn-8Zn-3Bi钎料时均大致为2.8~3.1；不同初始工艺条件对两种状态钎料/Cu焊点界面IMC生长速率的影响无明显差异；不同状态钎料对焊点固态时效过程中界面IMC生长动力学的影响不明显。
Sn-9Zn中添加0.1wt.%Cr后，钎料的铺展性能及钎料/Cu焊点结合强度明显改善，快速凝固态Sn-9Zn-0.1Cr钎料/Cu焊点界面IMC相对更为均匀，力学性能的提高更为显著；0.1wt.%Cr在Sn-9Zn中的添加能够减小钎料/Cu焊点固态时效过程中界面IMC的生长速率，对界面IMC在服役过程中的过度生长抑制作用明显。
微量稀土（RE）元素在Sn-9Zn合金中的添加具有明显变质作用，添加量较多时合金中所形成的RE化合物在局部的聚集会导致性能下降；Sn-9Zn合金中添加0.1wt.%RE元素Nd时，界面组织的均匀细化有利于改善焊点力学性能。
本课题的试验研究表明，快速凝固及微合金化技术在部分Sn-Zn系无铅钎料改性制备中的单一或复合应用，能够实现钎料/基板间在较低温度和/或较短时间工艺条件下即形成有效连接，能够抑制界面IMC的不利影响和改善接头组织与力学性能。本课题的研究拓宽了高性能Sn-Zn系无铅钎料的研究与应用范畴。
The development of lead-free solders has been an essential and urgent task in theelectronics packaging industry because of the restriction of lead use by legislations.Sn-Zn alloys, which have some advantages, such as relatively low melting point,cost-saving and superior mechanical property, is considered as one of candidates thatcould replace Pb-containing solders in microelectronic packaging and interconnects.However, because Zn element is quite active, Sn-Zn system solders have worse wettingand corrosion behavior. The high temperature oxidation resistance and embrittlementbehavior of the Sn-Zn alloys is also of low quality.
The subject aims at the questions existing in Sn-Zn alloys and studies the effect ofrapid solidification process and/or micro-alloying on microstructure and characteristicsof solder alloys. The interface behavior of solder/Cu and the mechanical properties ofsoldering joints are also investigated. The as-solidified eutectic Sn-Zn solder isemployed as the reference system.
The studies showed that a CuZn intermetallic compound (IMC) layer was formedpreferentially within the Cu substrate at the Sn-Zn/Cu interface and the Cu_5Zn_8IMCformed by the reaction of CuZn with Zn atoms diffused from the solder. The diffusionand aggregation of the Cu atoms which crossed the IMC layer into the solder presented“pulsation" in the form, and the granular Cu_5Zn_8IMCs were formed in the solder. TheIMC at the interface was present an appearance of three types: coarse IMC layer at theinterface, compact cellular Cu_5Zn_8layer, and tabular CuZn IMC layer.
Microstructure analysis of solder alloys showed that a netlike dendrite structure wasformed due to the rapid branch of β-Sn, the growth of Zn phases was suppressed anddistributed in β-Sn matrix in granular form with a size of0.5~2μm. By contrast to theas-solidified Sn-9Zn alloy, the addition of0.1wt.%Cr in Sn-9Zn alloy promoted thedissolution of Zn in Sn during the rapid solidification process. The microstructure of thesoldering seam was notably fined and the Zn phases were not distinctly greater than1μm. The Zn phases in rapidly solidified Sn-8Zn-3Bi presented granular or strip andblock pattern, with a size of2~4μm. Bi was completely dissolved in Sn and formedsupersaturated solid solution.
The analysis results of melting characteristic of various solder alloys indicated thatthe melting temperatures of Sn-9Zn and Sn-6.5Zn were almost not changed after rapid solidification. By contrast to the as-solidified alloys, after rapid solidification, themelting point of the Sn-9Zn-0.1Cr alloy was lower by about9°C and the Sn-8Zn-3Bisolder was rise by about7°C. The pasty range of rapidly solidified alloys obviouslydecreased. The metastable phase in the rapidly solidified alloys could release the crystallatent heat during the soldering process and then promote the fusion of the solder.
The analysis of IMC at the interface of Sn-Zn/Cu showed that the fine Zn phasesand precipitates in rapidly solidified solder promoted the homogeneity of the interfacialreaction. The Cu_5Zn_8intermetallics at the interface by using the rapidly solidifiedSn-9Zn alloy were finer and more uniform than that of the as-solidified Sn-9Zn alloy,and the tensile-shear strength of the joint was obviously improved.
As aging time prolonged at150°C, the thickness of the IMC layer changed from anincrease to a reduction and the continuity and compactability of this layer was destroyeddue to the decomposition of the Cu-Zn IMC layer. A discontinuous layer of Cu6Sn5IMC was present within the Cu substrate near the decomposed region. By comparisonwith as-solidified solders, the compact and uniform IMC layer at the interface by use ofthe rapidly solidified solder was more stable during aging at150°C.
The growth kinetics analysis of the interfacial IMC showed that the growth of IMCat the interface of solder/Cu during the soldering process could be suppressed due to asuitable addition of the elements Bi and Cr. In the tests, the growth rate constant k ofthe IMC at the interface of solder/Cu during soldering at240°C by using the Sn-9Znalloy and the Sn-9Zn-0.1Cr or Sn-8Zn-3Bi alloys was3.5,2.8~3.1, respectively. Theeffects of various initial process conditions on the growth rate were puny. The effects ofsolder state on the growth kinetics of the interfacial IMC during solid aging wereslightly.
The addition of0.1wt.%Cr in Sn-9Zn, the wettability and the bonding strength ofsolder/Cu were improved obviously. The IMC layer became relatively uniform and thetensile-shear strengths of the joints using the rapidly solidified solder were markedlyhigher than those of the joints using the as-solidified solders. The former exhibited goodsolderability and excellent joint strength. Due to the addition of0.1wt.%Cr in Sn-9Zn,the growth rate of the IMC was decreased during the solid aging process and theexcessive growth of the IMC layer at the interface can be suppressed.
The addition of minor rare earth (RE) elements in Sn-9Zn alloy has distinctmetamorphism, but the RE compounds could be formed due to the overmuch addition.The improved properties of the joints of the Cu/Sn-9Zn-0.1Nd/Cu might result from the formation of the uniform, fine-grained microstructure at the interface.
Studies in this project show that a suitable application of the rapid solidificationtechnology and alloying method independently or simultaneously can significantlyimprove the combination property of the Sn-Zn system lead-free solders. Then, thesoldering process can complete in a shorter period of time or/and a lower temperaturecompared with the as-solidified solders and the joints are of high quality. The adverseeffect of the IMC at the interface on the microstructure and mechanical properties issuppressed. The research extends the fields of the study and application of Sn-Znlead-free solder alloys with high-performance.
针对Sn-Zn系钎料合金所存在的问题，本文以共晶Sn-Zn无铅钎料作为参照物，研究了快速凝固及微合金化对Sn-Zn系钎料显微结构、合金特性、钎料/Cu界面行为及焊点力学性能的影响。
研究表明，Sn-Zn钎料/Cu焊点界面紧靠Cu基板侧形成CuZn金属间化合物（IMC）层，CuZn IMC有与钎料中的Zn原子继续反应生成Cu_5Zn_8的趋势；Cu原子越过Sn-Zn钎料/Cu基板界面IMC层向钎料中的扩散与聚集呈现“脉动”形式，并在邻近结合面的钎料中形成粒状Cu_5Zn_8IMC；Sn-Zn钎料与Cu基板界面IMC主要表现为3种形貌：粗糙的界面Cu_5Zn_8IMC层、致密的Cu_5Zn_8胞状晶层、板状CuZn IMC层。
合金微观分析表明，Sn-Zn钎料在本试验快速凝固条件下，初生β-Sn相快速生长与分枝形成网络状枝晶，Zn相的长大被抑制，呈尺寸为0.5~2μm的细小颗粒状被包覆于β-Sn枝晶中；与Sn-9Zn合金相比，0.1wt.%Cr的添加对基体组织的细化作用促进了快速凝固过程中Zn在Sn中的固溶，组织中β-Sn相枝晶更为均匀，颗粒状Zn相更为细小（尺寸基本上不大于1μm）且分布更为弥散；快速凝固态Sn-8Zn-3Bi合金中，Zn相以不规则的尺寸大致为2-4μm的细小条块状或颗粒状分布于Sn枝晶中，Bi均以过饱和固溶体形式存在于Sn相中。
钎料熔化特性分析结果表明，经本文工艺条件下快速凝固制备后，Sn-Zn合金的熔点几乎无变化，Sn-9Zn-0.1Cr合金的熔点降低约9°C，而Sn-8Zn-3Bi合金由于Bi完全固溶在Sn中导致熔点反而升高了约7°C；与常态合金相比，处于热力学亚稳定状态的快速凝固态Sn-Zn系合金熔化区间均显著减小，在钎焊加热过程中结晶潜热的释放促进了钎料对基板的润湿与铺展。
Sn-Zn/Cu界面IMC分析表明，快速凝固态钎料中细小的Zn相与析出相在钎焊过程中与基板元素间的反应均匀，避免了界面处粗大块状Cu_5Zn_8IMC的形成，能够促进钎焊时均匀界面反应层的形成，显著提高了焊点结合强度。
150°C长时间时效会导致Sn-Zn/Cu焊点界面Cu-Zn化合物的分解，IMC层厚度表现为随时间的延长先增大而后减小的趋势，局部被破坏的界面区Cu基体处形成Cu_6Sn_5化合物；与常态钎料相比，使用快速凝固态Sn-Zn钎料所形成的较为均匀致密的界面IMC层在高温时效过程中较稳定。
界面IMC生长动力学分析结果表明：适量合金元素Cr、Bi在Sn-9Zn合金中的添加能够抑制钎焊过程中界面Cu-Zn IMC的生长；本文试验条件下，钎焊温度为240°C时钎料/Cu基板钎焊过程中IMC生长速率常数k分别为：使用Sn-9Zn钎料时约为3.5，使用Sn-9Zn-0.1Cr或Sn-8Zn-3Bi钎料时均大致为2.8~3.1；不同初始工艺条件对两种状态钎料/Cu焊点界面IMC生长速率的影响无明显差异；不同状态钎料对焊点固态时效过程中界面IMC生长动力学的影响不明显。
Sn-9Zn中添加0.1wt.%Cr后，钎料的铺展性能及钎料/Cu焊点结合强度明显改善，快速凝固态Sn-9Zn-0.1Cr钎料/Cu焊点界面IMC相对更为均匀，力学性能的提高更为显著；0.1wt.%Cr在Sn-9Zn中的添加能够减小钎料/Cu焊点固态时效过程中界面IMC的生长速率，对界面IMC在服役过程中的过度生长抑制作用明显。
微量稀土（RE）元素在Sn-9Zn合金中的添加具有明显变质作用，添加量较多时合金中所形成的RE化合物在局部的聚集会导致性能下降；Sn-9Zn合金中添加0.1wt.%RE元素Nd时，界面组织的均匀细化有利于改善焊点力学性能。
本课题的试验研究表明，快速凝固及微合金化技术在部分Sn-Zn系无铅钎料改性制备中的单一或复合应用，能够实现钎料/基板间在较低温度和/或较短时间工艺条件下即形成有效连接，能够抑制界面IMC的不利影响和改善接头组织与力学性能。本课题的研究拓宽了高性能Sn-Zn系无铅钎料的研究与应用范畴。
The development of lead-free solders has been an essential and urgent task in theelectronics packaging industry because of the restriction of lead use by legislations.Sn-Zn alloys, which have some advantages, such as relatively low melting point,cost-saving and superior mechanical property, is considered as one of candidates thatcould replace Pb-containing solders in microelectronic packaging and interconnects.However, because Zn element is quite active, Sn-Zn system solders have worse wettingand corrosion behavior. The high temperature oxidation resistance and embrittlementbehavior of the Sn-Zn alloys is also of low quality.
The subject aims at the questions existing in Sn-Zn alloys and studies the effect ofrapid solidification process and/or micro-alloying on microstructure and characteristicsof solder alloys. The interface behavior of solder/Cu and the mechanical properties ofsoldering joints are also investigated. The as-solidified eutectic Sn-Zn solder isemployed as the reference system.
The studies showed that a CuZn intermetallic compound (IMC) layer was formedpreferentially within the Cu substrate at the Sn-Zn/Cu interface and the Cu_5Zn_8IMCformed by the reaction of CuZn with Zn atoms diffused from the solder. The diffusionand aggregation of the Cu atoms which crossed the IMC layer into the solder presented“pulsation" in the form, and the granular Cu_5Zn_8IMCs were formed in the solder. TheIMC at the interface was present an appearance of three types: coarse IMC layer at theinterface, compact cellular Cu_5Zn_8layer, and tabular CuZn IMC layer.
Microstructure analysis of solder alloys showed that a netlike dendrite structure wasformed due to the rapid branch of β-Sn, the growth of Zn phases was suppressed anddistributed in β-Sn matrix in granular form with a size of0.5~2μm. By contrast to theas-solidified Sn-9Zn alloy, the addition of0.1wt.%Cr in Sn-9Zn alloy promoted thedissolution of Zn in Sn during the rapid solidification process. The microstructure of thesoldering seam was notably fined and the Zn phases were not distinctly greater than1μm. The Zn phases in rapidly solidified Sn-8Zn-3Bi presented granular or strip andblock pattern, with a size of2~4μm. Bi was completely dissolved in Sn and formedsupersaturated solid solution.
The analysis results of melting characteristic of various solder alloys indicated thatthe melting temperatures of Sn-9Zn and Sn-6.5Zn were almost not changed after rapid solidification. By contrast to the as-solidified alloys, after rapid solidification, themelting point of the Sn-9Zn-0.1Cr alloy was lower by about9°C and the Sn-8Zn-3Bisolder was rise by about7°C. The pasty range of rapidly solidified alloys obviouslydecreased. The metastable phase in the rapidly solidified alloys could release the crystallatent heat during the soldering process and then promote the fusion of the solder.
The analysis of IMC at the interface of Sn-Zn/Cu showed that the fine Zn phasesand precipitates in rapidly solidified solder promoted the homogeneity of the interfacialreaction. The Cu_5Zn_8intermetallics at the interface by using the rapidly solidifiedSn-9Zn alloy were finer and more uniform than that of the as-solidified Sn-9Zn alloy,and the tensile-shear strength of the joint was obviously improved.
As aging time prolonged at150°C, the thickness of the IMC layer changed from anincrease to a reduction and the continuity and compactability of this layer was destroyeddue to the decomposition of the Cu-Zn IMC layer. A discontinuous layer of Cu6Sn5IMC was present within the Cu substrate near the decomposed region. By comparisonwith as-solidified solders, the compact and uniform IMC layer at the interface by use ofthe rapidly solidified solder was more stable during aging at150°C.
The growth kinetics analysis of the interfacial IMC showed that the growth of IMCat the interface of solder/Cu during the soldering process could be suppressed due to asuitable addition of the elements Bi and Cr. In the tests, the growth rate constant k ofthe IMC at the interface of solder/Cu during soldering at240°C by using the Sn-9Znalloy and the Sn-9Zn-0.1Cr or Sn-8Zn-3Bi alloys was3.5,2.8~3.1, respectively. Theeffects of various initial process conditions on the growth rate were puny. The effects ofsolder state on the growth kinetics of the interfacial IMC during solid aging wereslightly.
The addition of0.1wt.%Cr in Sn-9Zn, the wettability and the bonding strength ofsolder/Cu were improved obviously. The IMC layer became relatively uniform and thetensile-shear strengths of the joints using the rapidly solidified solder were markedlyhigher than those of the joints using the as-solidified solders. The former exhibited goodsolderability and excellent joint strength. Due to the addition of0.1wt.%Cr in Sn-9Zn,the growth rate of the IMC was decreased during the solid aging process and theexcessive growth of the IMC layer at the interface can be suppressed.
The addition of minor rare earth (RE) elements in Sn-9Zn alloy has distinctmetamorphism, but the RE compounds could be formed due to the overmuch addition.The improved properties of the joints of the Cu/Sn-9Zn-0.1Nd/Cu might result from the formation of the uniform, fine-grained microstructure at the interface.
Studies in this project show that a suitable application of the rapid solidificationtechnology and alloying method independently or simultaneously can significantlyimprove the combination property of the Sn-Zn system lead-free solders. Then, thesoldering process can complete in a shorter period of time or/and a lower temperaturecompared with the as-solidified solders and the joints are of high quality. The adverseeffect of the IMC at the interface on the microstructure and mechanical properties issuppressed. The research extends the fields of the study and application of Sn-Znlead-free solder alloys with high-performance.
引文
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