Sn-Cu-Bi合金液—液结构转变及其对凝固和钎焊性的影响
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摘要
近年来,压力或温度诱导液-液结构转变现象的发现打破了液态结构和性质连续渐变的传统认知,深入认识液-液结构转变的物理本质及其规律,对认识液态金属与合金的本质以及新材料的开发无疑具有重要的意义。目前,对无铅钎料的研究和开发仍然局限于成分选择、配比优化及微量元素的影响等方面,很少有人关注熔体热历史对无铅钎料组织和性能的影响。
本文以Sn-0.7Cu-xBi合金(Bi质量分数分别为0%,3%,5%,7.5%和10%)为研究对象,从温度诱导的液-液结构转变这一新视角出发,探索了熔体结构状态变化及其与无铅钎料组织和性能的相关性,同时考察了Bi元素对Sn-0.7Cu钎料组织和钎焊性的影响。主要研究内容及结果如下:
(1)采用直流四电极法研究了熔化过程中Sn-0.7Cu-xBi合金电阻率—温度关系,结果显示Bi的添加降低了合金熔点,同时增大了熔程;而随后连续两轮升、降温的电阻率—温度曲线均出现了异常变化,并在第一轮升温后表现出可逆转变特征。
(2)通过实验探讨了Bi含量、液液结构转变对凝固的影响,发现Bi含量越高,Sn-0.7Cu-xBi合金凝固组织中β-Sn和富Cu相越细小;经历液-液结构转变的Sn-0.7Cu-xBi合金其凝固组织更加均匀、细小。
(3)将由铁模凝固实验所得钎料试样在铜板上进行铺展实验。结果显示Bi的加入提高了Sn-Cu(Bi)钎料的润湿性能,尤其是Bi含量在0～3%时;液-液结构转变对Sn-0.7Cu合金润湿性的影响较为显著。
(4)对铺展实验试样在150℃下进行了0,120,240,480h的时效处理。接头组织观察表明,Bi的添加增大了钎焊态下界面IMC的晶粒尺寸,却抑制了时效过程中IMC的生长;液-液结构转变后的Sn-Cu(Bi)钎料/Cu界面IMC的形成和生长均受到了抑制。
(5)采用单剪搭接接头形式,对Sn-Cu(Bi)钎料/Cu接头剪切强度进行了测试,结果表明,随Bi含量的增加接头剪切强度先增大,后减小,Bi含量在3%时最大;在Bi含量相同时,液-液结构转变提高了钎料本身接头剪切强度。综合看经历液-液结构转变的Sn-0.7Cu-3Bi钎料的综合钎焊性最好。
In recent years, pressure or temperature-induced liquid-liquid structure transitions (L-LSTs) have been found in liquids, which challenge our conventional picture of liquid as entity with a continuously varying averaged structure. In-depth investigation on the nature and rule of L-LSTs is of significance to understand the structure of liquid substance and to develop new materials. So far, the studies on lead-free solders materials mainly focus upon the selection of components and their optimization of the mixture ratio, and the influence of minor elements on various properties. Little attention has been paid to the effect of the melt heat history on the microstructures and properties of lead-free solders.
In this paper, Sn-0.7Cu-xBi (x=0, 3, 5, 7.5, 10 wt %) lead-free solders have been chosen as the investigation object. From the new viewpoint of temperature induced L-LST, the effect of L-LST on microstructures and soldering properties of Sn-0.7Cu-xBi are investigated. Besides, the effect of Bi on the microstructure and solderability of Sn-0.7Cu solders is studied. The main contents and conclusions are as follows:
(1) Temperature dependence of electrical resistivities of Sn-0.7Cu-xBi solders has been surveyed by the DC four-probe method. The results show that the addition of Bi in the Sn-0.7Cu solder decreases melting point while increases the melting temperature range. And the anomalous changes can be observed on the resistivity-temperature (ρ-T) curves at certain temperature ranges in two experimental cycles, and the anomalous changes are reversible after the first cycle heating.
(2) The effect of Bi and L-LST on the microstructures of Sn-Cu-Bi solders has been investigated by solidification experiments. It is found thatβ-Sn and Cu-rich phase become finer with the increase of Bi. Moreover, the microstructures become more homogeneous and finer after the melts have experienced L-LST.
(3) Spreadability tests of the iron-mold solidified sample on Cu substrate have been carried out. The results show that the addition of Bi can improve the wettability of Sn-Cu(Bi) solders, especially the addition of 0～3 wt %Bi. And the effect of L-LST on the wettability of Sn-0.7Cu solder is more obvious.
(4) The consequent thermal aging treatment for the solder joint has been performed at the temperature of 150℃for 0, 120, 240 and 480 h. The results show that the addition of Bi increases the size of Cu-Sn IMC in as-soldered joints, but inhibits the development of Cu-Sn IMC layer in thermally aged solder joints; while L-LST restrains the nucleation and development of Cu-Sn IMC.
(5) The shear strength of soldered lap-joint specimen has been measured. The results show that the shear strength of Sn-0.7Cu-xBi solders/Cu joints firstly increases and then decreases with the increase of Bi, and reaches the maximum strength at 3wt%Bi. L-LST enhances the shear strength of Sn-Cu(Bi) soldered joints. In general, Sn-0.7Cu-3Bi solder experienced L-LST has the best comprehensive properties.
本文以Sn-0.7Cu-xBi合金(Bi质量分数分别为0%,3%,5%,7.5%和10%)为研究对象,从温度诱导的液-液结构转变这一新视角出发,探索了熔体结构状态变化及其与无铅钎料组织和性能的相关性,同时考察了Bi元素对Sn-0.7Cu钎料组织和钎焊性的影响。主要研究内容及结果如下:
(1)采用直流四电极法研究了熔化过程中Sn-0.7Cu-xBi合金电阻率—温度关系,结果显示Bi的添加降低了合金熔点,同时增大了熔程;而随后连续两轮升、降温的电阻率—温度曲线均出现了异常变化,并在第一轮升温后表现出可逆转变特征。
(2)通过实验探讨了Bi含量、液液结构转变对凝固的影响,发现Bi含量越高,Sn-0.7Cu-xBi合金凝固组织中β-Sn和富Cu相越细小;经历液-液结构转变的Sn-0.7Cu-xBi合金其凝固组织更加均匀、细小。
(3)将由铁模凝固实验所得钎料试样在铜板上进行铺展实验。结果显示Bi的加入提高了Sn-Cu(Bi)钎料的润湿性能,尤其是Bi含量在0～3%时;液-液结构转变对Sn-0.7Cu合金润湿性的影响较为显著。
(4)对铺展实验试样在150℃下进行了0,120,240,480h的时效处理。接头组织观察表明,Bi的添加增大了钎焊态下界面IMC的晶粒尺寸,却抑制了时效过程中IMC的生长;液-液结构转变后的Sn-Cu(Bi)钎料/Cu界面IMC的形成和生长均受到了抑制。
(5)采用单剪搭接接头形式,对Sn-Cu(Bi)钎料/Cu接头剪切强度进行了测试,结果表明,随Bi含量的增加接头剪切强度先增大,后减小,Bi含量在3%时最大;在Bi含量相同时,液-液结构转变提高了钎料本身接头剪切强度。综合看经历液-液结构转变的Sn-0.7Cu-3Bi钎料的综合钎焊性最好。
In recent years, pressure or temperature-induced liquid-liquid structure transitions (L-LSTs) have been found in liquids, which challenge our conventional picture of liquid as entity with a continuously varying averaged structure. In-depth investigation on the nature and rule of L-LSTs is of significance to understand the structure of liquid substance and to develop new materials. So far, the studies on lead-free solders materials mainly focus upon the selection of components and their optimization of the mixture ratio, and the influence of minor elements on various properties. Little attention has been paid to the effect of the melt heat history on the microstructures and properties of lead-free solders.
In this paper, Sn-0.7Cu-xBi (x=0, 3, 5, 7.5, 10 wt %) lead-free solders have been chosen as the investigation object. From the new viewpoint of temperature induced L-LST, the effect of L-LST on microstructures and soldering properties of Sn-0.7Cu-xBi are investigated. Besides, the effect of Bi on the microstructure and solderability of Sn-0.7Cu solders is studied. The main contents and conclusions are as follows:
(1) Temperature dependence of electrical resistivities of Sn-0.7Cu-xBi solders has been surveyed by the DC four-probe method. The results show that the addition of Bi in the Sn-0.7Cu solder decreases melting point while increases the melting temperature range. And the anomalous changes can be observed on the resistivity-temperature (ρ-T) curves at certain temperature ranges in two experimental cycles, and the anomalous changes are reversible after the first cycle heating.
(2) The effect of Bi and L-LST on the microstructures of Sn-Cu-Bi solders has been investigated by solidification experiments. It is found thatβ-Sn and Cu-rich phase become finer with the increase of Bi. Moreover, the microstructures become more homogeneous and finer after the melts have experienced L-LST.
(3) Spreadability tests of the iron-mold solidified sample on Cu substrate have been carried out. The results show that the addition of Bi can improve the wettability of Sn-Cu(Bi) solders, especially the addition of 0～3 wt %Bi. And the effect of L-LST on the wettability of Sn-0.7Cu solder is more obvious.
(4) The consequent thermal aging treatment for the solder joint has been performed at the temperature of 150℃for 0, 120, 240 and 480 h. The results show that the addition of Bi increases the size of Cu-Sn IMC in as-soldered joints, but inhibits the development of Cu-Sn IMC layer in thermally aged solder joints; while L-LST restrains the nucleation and development of Cu-Sn IMC.
(5) The shear strength of soldered lap-joint specimen has been measured. The results show that the shear strength of Sn-0.7Cu-xBi solders/Cu joints firstly increases and then decreases with the increase of Bi, and reaches the maximum strength at 3wt%Bi. L-LST enhances the shear strength of Sn-Cu(Bi) soldered joints. In general, Sn-0.7Cu-3Bi solder experienced L-LST has the best comprehensive properties.
引文
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