Bi Layer Formation at the Anode Interface in Cu/Sn 58Bi/Cu Solder Joints with High Current Density

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1 J. Mater. Sci. Technol., 2012, 28(1), Bi Layer Formation at the Anode Interface in Cu/Sn 58Bi/Cu Solder Joints with High Current Density Hongwen He 1), Haiyan Zhao 1), Fu Guo 2) and Guangchen Xu 2) 1) Department of Mechanical Engineering, Tsinghua University, Beijing , China 2) College of Materials Science and Engineering, Beijing University of Technology, Beijing , China [Manuscript received June 8, 2010, in revised form September 6, 2010] Bi layer formation in Cu/Sn 58Bi/Cu solder joints was investigated with different current densities and solder thickness. Uniform and continuous Bi layers were formed at the anode interface which indicated that Bi was the main diffusing species migrating from the cathode to the anode. The electromigration force and Joule heating took on the main driving forces for Bi diffusion and migration. In addition, two appearance types of Bi layers, planar-type and groove-type, were found during current stressing. The morphology and thickness of Bi layers were affected by current density and current stressing time. KEY WORDS: Bi layer formation; Current density; Electromigration; Joule heating 1. Introduction As electronic industry continues to pursuit high performance and the miniaturization of electronic devices, the demand for high current density may cause failures in solder joints. Each solder joint is designed to carry 0.2 A which means that the average current density through a solder joint may exceed 10 4 A/cm 2 or much higher [1,2]. Therefore, electromigration (EM) issues increasingly become the substantial concern in electronic packaging. Meanwhile, since Joule heating is proportional to the square of the current density, the local temperature of conductive lines and solder joints will rise substantially. The solder joints will experience a temperature rise of at least 100 C [3]. As a consequence, under the combined effect of a high current density and a high homologous temperature, easy diffusion of atoms in the lattice is anticipated. EM is commonly defined as mass transport due to momentum exchange between conducting electrons and diffusing metal atoms when a high current density is applied. Metal atoms diffuse along the direction of electron flux, which results in the voids or cracks formation at the cathode side and hillocks formation Corresponding author. Ph.D.; Tel.: ; address: hehongwen@mail.tsinghua.edu.cn (H.W. He). at the anode side [4,5]. Sn Bi lead-free solder has been considered as one of the most promising lead-free products as a substitute for conventional SnPb solders in recent years. Its low melting point makes it widely used in some special situation for soldering [6,7]. As one of the most excellent lead-free solders, its reliability issues are being paid much more attention. It is a simple eutectic system with a eutectic composition of 42 wt% Sn and 58 wt% Bi that melts at 138 C. Sn has almost no solubility in Bi. As we all know that in eutectic twophase solder joints, phase separation is likely to occur under EM due to different atomic diffusivities over a range of operational temperatures. It was found that Sn and Pb are the dominant diffusing species during EM in eutectic Sn37Pb solder joint at room temperature and above 100 C, respectively [8]. For the similar microstructure with Sn37Pb solder, phase separation is possible to occur under EM in Sn 58Bi solder matrix. Chen et al. [9,10] has reported the Bi accumulation phenomenon at the anode side due to EM which seriously degrades the solder joint reliability because of its brittleness property. This paper mainly investigated the Bi segregation at the anode side during EM process with different current densities and solder thickness.

2 H.W. He et al.: J. Mater. Sci. Technol., 2012, 28(1), Fig. 1 Schematic drawing and the geometric dimension of the Cu/Sn 58Bi/Cu solder joint 2. Experimental The preparation procedure of the Cu/Sn 58Bi/Cu solder joints includes five steps: alloy smelting, solder balls production, soldering, inlaying and polishing. First of all, pure Sn and Bi metal particles with purity of 99.9 wt% were used as raw materials. Sn and Bi metal particles were weighed accurately according to the mix percentage and then put into an Al 2 O 3 ceramic crucible, and meanwhile eutectic salt (KCl+LiCl) with weight ratio of 1.3:1 was used to cover the surface of the particles to prevent oxidation during smelting. The crucibles were placed in an induction furnace at 550 C for about 20 min. The molten alloy was then held on for about 40 min and mechanically stirred every 10 min with a glass rod to promote uniformity of the solder alloy [11,12]. The molten solder was finally chill cast into a rod ingot in a mold. Solder balls were made of solder alloy with uniform droplet spraying equipment in our laboratory. Solder balls were placed between two copper wires with 500 µm in diameter and placed on a hot plate fixed in the soldering platform designed and built by authors. The specific soldering procedure was described in detail in our previous study [13 15]. Fig. 1 shows the schematic drawing and the geometric dimension of the Cu/Sn 58Bi/Cu solder joint. Unlike the line-to-bump geometry of a flip chip solder joint, the end-to-end structure has a very uniform current density distribution throughout the solder joint due to the special one-dimensional configuration. The current crowding taking place at the electron entry and exit region can be eliminated effectively. However, the Joule heating induced by high current stressing will still affect the EM reliability. Therefore, the heat dissipation plate made of aluminium was installed on the solder joint and together mounted with epoxy resin to dissipate the Joule heating. A grinding machine was applied to reduce the dimension of the samples, followed by grid sandpapers, and finely polished with Al 2 O 3 suspension. Microstructural and compositional analysis was examined by using an S-3400N scanning electron microscope (SEM) equipped with an energy dispersive Fig. 2 Apparatuses of the electromigration test: 1 MVC2000 camera, 2 microscope, 3 DC power supply, 4 sample X-ray spectroscopy system. After sample preparation, the electromigration test would be conducted under a stable circumstance. The sample was fixed on a plate and connected with a DC power supply to provide a constant current flow. For convenient observation, a Microview MVC 2000 camera was mounted on the optical microscope equipped with a relevant software to monitor and record the test process. Fig. 2 shows apparatuses of the electromigration test monitoring with the Microview MVC 2000 camera. The average current density is calculated vis dividing the current value by the virtual cross sectional area through which the electrons pass. In this work, the samples were stressed with the current density of A/cm 2 at 80 C and 10 4 A/cm 2 at room temperature, respectively. 3. Results and Discussion 3.1 Bi layer formation Fig. 3 shows a typical uniform two-phase microstructure of the as-soldered Cu/Sn 58Bi/Cu solder joint before current stressing, the white Bi phase and the gray Sn phase, where Fig. 3(a) and (b) represent the microstructure at the cathode side and the anode side, respectively. The direction of the current flow is from the anode to the cathode, but the direction of the electrons is on the contrary. Depending on the experimental condition with the same current density of A/cm 2 at 80 C, two samples were employed with the different solder thickness of 300 and 150 µm. Fig. 4 shows the microstructural evolution at the anode interface of the Cu/Sn 58Bi/Cu solder joint with the solder thickness of 300 µm after current stressing for 540, 630 and 720 h, respectively. Fig. 4(d) is the locally enlarged image of Fig. 4(c). Compared with the microstructure prior to current stressing, obvious changes occur in the solder matrix. The original uniform two phase microstructure was disturbed with increasing current stressing time. The most interesting phenomenon was that a uniform Bi layer was found at the anode

3 48 H.W. He et al.: J. Mater. Sci. Technol., 2012, 28(1), Fig. 3 Microstructural morphologies of the as-soldered Cu/Sn 58Bi/Cu solder joint: (a) at the anode, (b) at the cathode interface. In order to concentrate on the microstructural analysis of the Bi layer formation, the local region of the anode was observed and analyzed. It is clearly seen from Fig. 4(a) that a uniform Bi layer is formed at the anode interface with the average thickness of 6.5 µm when the current stressing time is 540 h. The structure of the Bi layer is not very compact and displays a groove-type appearance, which seems that the Bi layer is inlaid into the solder matrix. Furthermore, many stripes are attached on the Bi layer surface as can be clearly seen in Fig. 4(d). Bi accumulation appears at some local regions between the Bi layer and the solder matrix. It should be noted that many intermetallic compounds (IMCs) grains distribute along the anode interface between Bi layer and Cu substrate. In addition, some large laminar IMCs are formed on the Cu substrate. Energy dispersive X-ray spectroscopy (EDS) compositional results indicate that these IMCs are Cu 6 Sn 5. With the increase of stressing time up to 630 and 720 h, the Bi layer thicknesses increase correspondingly as can be seen in Fig. 4(b) and (c). The average Bi layer thickness as a function of stressing time is plotted in Fig. 5. As the stressing time reaches 630 h, the Bi layer thickness is 14.5 µm, which increases by 8 µm in 90 h. However, when the stressing time continues to reach 720 h, the Bi layer thickness is 17.5 µm, which increases only by 3 µm during the same stressing time. In other words, the Bi layer thickness increases rapidly at the initial stage and then increases slowly when the stressing time continues. To confirm the composition of the microstructure, EDS compositional analysis experiments were performed after the current stressing. As shown in Fig. 4(c), marked regions A to D, and the corresponding results are Fig. 4 Microstructural morphologies of the Cu/Sn 58Bi/Cu solder joint with the current density of A/cm 2 at 80 C at the anode interface after current stressing: (a) 540 h, (b) 630 h, (c) 720 h, (d) 720 h

4 H.W. He et al.: J. Mater. Sci. Technol., 2012, 28(1), Thickness / m Stressing time / h Fig. 5 Average Bi layer thickness as a function of stressing time at the anode interface Table 1 EDS results of zones A D in Fig. 4(c) Region Bi Sn Cu A B C D shown in Table 1. As the solder thickness is reduced to 150 µm, the growth rate of Bi layer is accelerated with the same current density and temperature circumstance. Fig. 6 illustrates the local microstructural evolution of the Cu/Sn 58Bi/Cu solder joint with solder thickness of 150 µm after current stressing for 114 h, where Fig. 6(a) and (c) represent the microstructure at the cathode and Fig. 6(b) and (d) represent the microstructure at the anode. Results show that the solder surface is protruded rather than smooth after the current stressing. Obvious two-phase separation occurs throughout the whole solder matrix. Most of Sn accumulates at the cathode and Bi aggregates at the anode interface to form a continuous Bi extrusion as can be seen in Fig. 6(a) and (b). Fig. 7 presents the element mapping of Sn and Bi in Fig. 6(b) which further proves the former deduction. In order to clarify the interior microstructure evolution, the solder joint was polished with Al 2 O 3 suspension. As shown in Fig. 6(c) and (d), an evident crack is found at the cathode interface. A majority of Bi atoms have accumulated at the anode interface to form a continuous and uniform Bi layer with the average thickness of 13.3 µm. Between the Bi layer and Cu substrate, a Cu 6 Sn 5 IMC layer is also found with the average thickness of 2.2 µm. Although two phase segregation occurs, many tiny Bi particles are still uniformly dispersed in the Sn-rich matrix with two appearance types, granular type and zonal type. Another EM experiment was performed with higher current density of 10 4 A/cm 2 at room temperature. Fig. 8 shows the microstructural evolution at the anode interface of the Cu/Sn 58Bi/Cu solder joint after current stressing for 92 h, where Fig. 8(a) Fig. 6 Microstructural morphologies of Cu/Sn 58Bi/Cu solder joint with current density of A/cm 2 at 80 C after current stressing for 114 h: (a) and (c) at the cathode, (b) and (d) at the anode. (a) Sn aggregation at the cathode after EM test, (b) Bi extrusion at the cathode after EM test, (c) crack formaion at the cathode after polishing, (d) Bi layer formation at the anode after polishing

5 50 H.W. He et al.: J. Mater. Sci. Technol., 2012, 28(1), Fig. 7 Element mapping of Sn and Bi in Fig. 6(b) and (c) represent the microstructure at the cathode and Fig. 8(b) and (d) represent the microstructure at the anode, respectively. Because the current density increases twice to 10 4 A/cm 2, the Bi layer formation at the anode interface is accelerated as the current stressing time reaches 92 h. As can be seen from Fig. 8(b) and (d), a thick Bi layer is formed at the anode interface with the average thickness of 10 µm. The appearance is very different from that of the sample stressed with the current density of A/cm 2. It is composed of compact Bi atoms to form a planar Bi layer and no grooves and stripes are found on the Bi layer surface. Furthermore, cracks and voids are formed at the cathode interface as shown in Fig. 8(a) and (c). 3.2 Phase coarsening Another noticeable phenomenon of the microstructural evolution in the solder matrix is the different phase coarsening at the cathode and anode side. It should be noted that the size of the Bi grains at the anode interface and cathode interface was not consistent any more compared with that of before current stressing. In other words, the growth of the Bi grains at the two sides was influenced after the sample was stressed with a higher current density. To quantify the Bi grains evolution at the two interfaces, a set of scientific software named Image J was employed. Here, how to conduct the image disposal process was briefly introduced. First of all, a 30 µm 30 µm square area should be cropped from the selected original image. Afterwards, the threshold with black and white item was adjusted to obtain the image as can be seen in Fig. 9(a) and (c). And then the analyze particles item was used to quantify the Bi grains. Before counting and measuring objects, the particle analyzer should be configured. By entering a single value, Fig. 8 Microstructural morphologies of the Cu/Sn 58Bi/Cu solder joint with current density of 10 4 A/cm 2 at room temperature after current stressing for 92 h: (a) and (c) at the cathode, (b) and (d) at the anode

6 H.W. He et al.: J. Mater. Sci. Technol., 2012, 28(1), Fig. 9 Bi-rich phase distribution obtained by Image J software Table 2 Bi layer thicknesses with different current density and solder thickness Sample Solder thickness/µm Current density/(a/cm 2 ) Stressing time/h Bi layer thickness/µm A B C particles smaller than this value can be ignored. Accordingly, the profiles of the Bi grain size at the anode and cathode interfaces after current stressing were obtained as shown in Fig. 9(b) and (d), respectively. Under such conditions, the average size of the Bi grain was calculated to be 3.05 and 1.04 µm 2 at the anode and cathode interfaces, respectively. From the results, it was concluded that the Bi grains at the anode grew and coarsened greater than that of at the cathode with the increase of the current stressing time. Therefore, it was proposed that the Bi-rich phase coarsening at the anode was enhanced by the current stressing as a result of enhanced diffusion related to an elevated temperature and atomic stimulation. 3.3 Mechanism of Bi layer formation According to the above EM tests in the Cu/Sn 58Bi/Cu solder joints stressed with different current densities of and A/cm 2, it can be deduced that the Bi layer formation at the anode interface depends on many factors, such as current density, stressing time, Joule heating, solder thickness, chemical gradients and so on. In the opinion of the present authors, current density and Joule heating take on the main driving force for the Bi layer formation. Comparison of Bi layer thickness under different experiment condition is summarized in Table 2. When the sample is stressed with the current density of A/cm 2 at 80 C, the Bi layer thickness increases rapidly at the initial stressing period and then slows down the increasing pace. Furthermore, the Bi layer thickness reaches 13.3 µm only after current stressing for 114 h under the same EM condition as the solder thickness reduces to 150 µm. That is to say that the solder thickness also has

7 52 H.W. He et al.: J. Mater. Sci. Technol., 2012, 28(1), great influence on the Bi layer formation at the anode interface. Another conclusion can also be analyzed that higher current density accelerates the Bi layer growth. Based on the above experimental results, Bi is the main diffusion species rather than Sn during the EM process. As Bi and Sn atoms are forced to depart from their equilibrium positions, it is expected to cause compressive stress in the direction of the electron flow and produce tensile stress in an upstream direction with respect to the electron flow. With increasing current stressing time, the Bi phases act as the main diffusing species at the initial duration. When they reach the anode, compressive stress forms due to the superfluous atomic flux [16,17]. Therefore, the stress gradient comes into being near the anode region. Consequently, the Bi layer formation is produced at the anode interface due to the departure of Sn atoms. Some investigators presented the movement of Sn and Pb during the early stage of current stressing in Sn Pb solder which indicated that initially both Sn and Pb migrated toward the anode as a consequence of EM [18]. This is strongly in accordance with the result presented in our experiment that Bi and Sn atoms are forced to move towards the anode at the beginning of the EM test. However, because the different physical properties of Sn and Bi, such as resistivity, heat expansion coefficient, and atomic number and so on, all affect the movement velocity of the metal atoms, Bi travels faster than Sn and first arrives at the anode to gradually form a continuous layer as the current stressing time increases. Besides the influence of current density which drive Bi atoms to diffuse along the electron direction, Joule heating, as another important factor, should be considered. Although the end-to-end structure is designed to eliminate the Joule heating accumulation, however, as the current stressing time increases, some defects such as voids or cracks will appear at the solder interfaces, which will change the local current density distribution and lead to the local Joule heating accumulation. This will inevitably lead to a considerable temperature gradient across the solder joints, which can provide a driving force for atomic diffusion to trigger thermomigration. Bi layer formation at the anode interface will degrade the mechanical reliability of the solder joint for its brittleness character. Chen et al. [9] had proved that doping with Cu could retard the phase coarsening of the SnBi solder under current stressing. The coarsening rate was significantly reduced from 4.6 to 1.4 µm 3 /h when 1 wt% Cu was added. Also, they investigated the effect of a 0.5 wt% Ag addition on the EM behavior. It was found that some platelike Ag 3 Sn precipitates were formed inside the solder, and behaved as obstacles that intercepted the atomic migration [10]. Therefore, it is very important to investigate the EM behavior of the eutectic SnBi solder and understand the mechanism of Bi diffusion under current stressing, which provides a valuable insight to enhance the solder reliability. 4. Conclusion In this work, the mechanism of Bi layer formation at the anode interface in Cu/Sn 58Bi/Cu solder joints with the current density of and A/cm 2, and the solder thickness of 300 and 150 µm have been investigated, respectively. Results indicate that during EM process, Bi is the main diffusing species which migrates from the cathode side to the anode side to form a continuous Bi layer. The current densities and Joule heating take on the main driving force for Bi diffusion and migration. With the increase of current density and stressing time, the Bi layer thickness increases accordingly. Furthermore, solder thickness is another significant factor to affect the Bi layer formation. Acknowledgements This study is supported by the China Postdoctoral Science Foundation (No ), the Beijing Natural Science Foundation Program and Scientific Research Key Program of Beijing Municipal Commission of Education (No. KZ ). REFERENCES [1 ] Y.C. Chan and D. Yang: Prog. Mater. Sci., 2010, 55, 428. [2 ] G.E. Ice and B.C. Larson: Adv. Eng. Mater., 2000, 10, 643. [3 ] F. Cheng, H. Nishikawa and T. Takemoto: J. Mater. Sci., 2008, 43, [4 ] Q.T. Huynh, C.Y. Liu, C. Chen and K.N. Tu: J. Appl. Phys., 2001, 89, [5 ] A.T. Wu, C.N. Siao, C.S. Ku and H.Y. Lee: J. Mater. Res., 2010, 25, 2 [6 ] C.M. Chen and C.C. Huang: J. Alloy. Compd., 2007, 461, 235. [7 ] C.Y. Liu, C. Chen, C.N. Liao and K.N. Tu: Appl. Phys. Lett., 1999, 75, 58. [8 ] H. Gan and K.N. Tu: J. Appl. Phys., 2005, 97, [9 ] C.M. Chen and C.C. Huang: J. Mater. Res., 2008, 23, [10] C.M. Chen, C.C. Huang and C.N. Liao: J. Electron. Mater., 2007, 36, 760. [11] Z.G. Chen, Y.W. Shi, Z.D. Xia and Y.F. Yan: J. Electron. Mater., 2002, 31, [12] Z.G. Chen: Study on the Creep Behavior of SnAgCuRE Solder Joints, Ph.D. Thesis, Beijing University of Technology, (in Chinese) [13] G.C. Xu, H.W. He and F. Guo: J. Electron. Mater., 2009, 38, 273. [14] H.W. He, G.C. Xu, H. Hao and F. Guo: ICEPT, Shanghai, China, 2007, 225. [15] F. Guo, G.C. Xu and H.W. He: J. Mater. Sci., 2009, 44, [16] B.H.L. Chao, X.F. Zhang, S.H. Chae and P.S. Ho: Microelectron. Reliab., 2009, 49, 253. [17] J.W. Nah, K.W. Paik, J.O. Suh and K.N. Tu: J. Appl. Phys., 2003, 94, [18] S.W. Chen, C.M. Chen and W.C. Liu: J. Electron. Mater., 1998, 27, 1193.

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