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1 Microelectronic Engineering 86 (2009) Contents lists available at ScienceDirect Microelectronic Engineering journal homepage: Effect of small Sn 3.5Ag 0.5Cu additions on the structure and properties of Sn 9Zn solder in ball grid array packages Asit Kumar Gain a, Y.C. Chan a, *, Ahmed Sharif a, Winco K.C. Yung b a Department of Electronic Engineering, City University of Hong Kong, Tat Chee Avenue, Kowloon Tong, Hong Kong b Department of Industrial and Systems Engineering, The Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong article info abstract Article history: Received 25 July 2008 Received in revised form 20 February 2009 Accepted 10 April 2009 Available online 19 April 2009 Keywords: Microstructure Ball grid array solder joints Shearing force Sn 9Zn with various additions of Sn 3.5Ag 0.5Cu powder was prepared by mechanically dispersing different weight percentages (1, 3, 5 and 7) of Sn Ag Cu powder into Sn 9Zn solder paste. In the Sn Zn solder, scallop-shaped AuZn 3 intermetallic compound was found at the interfaces. On the other hand, in the Sn 3.5Ag 0.5Cu content solders, an additional e-agzn 3 intermetallic compound layer was found to be well adhered on the top surface of the AuZn 3 layer and the e-agzn 3 layer thickness increased with the number of reflow cycles. In addition, fine spherical-shaped e-agzn 3 intermetallic compound particles as well as an acicular-shaped Zn-rich phase was clearly observed in the b-sn matrix. On increasing the Sn Ag Cu content, the shear load was increased from 1.80 to 2.03 kg after one reflow cycle. In the Sn 3.5Ag 0.5Cu content solders, the fracture surfaces exhibited typical ductile behavior with very rough dimpled surfaces while the fracture surface in the Sn Zn solder gave fractures with a brittle appearance. In the fracture surface of the Sn 3.5Ag 0.5Cu content solders, some dimples were clearly observed associated with the formation of spherical-shaped e-agzn 3 intermetallic compound particles. Ó 2009 Elsevier B.V. All rights reserved. 1. Introduction Due to the environmental and health concerns of lead toxicity generated by conventional Sn Pb solder in the electronics industry [1 4], the search for a good Pb-free solder which is an environmentally friendly material is an important issue. Many Sn-based solders such as Sn Ag, Sn Cu, Sn Zn, Sn Ag Cu etc. have been developed as candidates for lead-free solders. Among them, Sn Zn solder has recently been considered as a suitable candidate for a Pb-free solder material because of its low melting point (198 C) as compared with other Sn-based solders e.g. Sn Cu (227 C), Sn Ag (221 C), Sn Ag Cu (217 C) as well as its low cost [5 7]. In general, the higher melting temperature, in the range of C associated with solders (Sn Cu (227 C), Sn Ag (221 C)), can damage the other electronic components mounted on the circuit board while reflowing [8]. However, some important issues such as inferior wettability, easy oxidation and micro-void formation need resolving to increase the practical use of these solder alloys [9 11]. Hence, much research has been concentrated on the addition of other elements into the Sn Zn solder so as to obtain better solder alloys and controlled fine microstructure. Development of new electronic devices especially using ball grid array (BGA) substrates and flip chips demands better solder * Corresponding author. Tel.: ; fax: address: eeycchan@cityu.edu.hk (Y.C. Chan). joint performance such as excellent wettability, a suitable melting temperature, good mechanical properties, good resistance to mechanical and thermal fatigue, corrosion resistance, good electrical properties, benign to health and the environment, ready availability and low material cost [12]. One innovative, potentially viable and economically affordable approach, to stabilize a fine grain microstructure, give homogeneous solder joint deformation as well as improving the mechanical properties of a solder, is the addition of an appropriate secondary phase as a reinforcement to a solder matrix so as to form a composite solder. Mohan et al. [13] prepared Sn Pb composite solders by the addition of single wall carbon nanotubes (SWCNT) as a reinforcing agent and their mechanical properties such as hardness, yield strength and ultimate tensile strength were shown to be superior to the unreinforced solder, while the melting point was not appreciably altered. Thus, several research groups have focused on the addition of secondary phases into lead-free solder matrices to form composite solders which is seen as an innovative approach to prepare leadfree composite solders with good mechanical properties. McCormack et al. [14] found that 1 wt% addition of Zn into a Sn 3.5 wt% Ag eutectic solder matrix gave a composite solder which was shown to improve the solidification microstructure of the Sn 3.5 wt% Ag eutectic solder by eliminating the large b-sn dendritic grains and introduced a finer and more uniform two phase distribution throughout the alloy. In addition, Fawzy [15] found that a 1 wt% Zn addition could increase the yield stress and /$ - see front matter Ó 2009 Elsevier B.V. All rights reserved. doi: /j.mee
2 2348 A.K. Gain et al. / Microelectronic Engineering 86 (2009) ultimate tensile stress of a Sn 3.5 wt% Ag solder. Guo et al. [16] reported that Ni reinforced Sn 3.5Ag/Ni composite solders improved the mechanical properties without significantly altering the wetting characteristics, microstructure and IMC layer growth of eutectic a Sn 3.5Ag solder. In the present study as a new approach, Sn 9Zn with various additions of Sn 3.5Ag 0.5Cu powder was prepared by mechanically dispersing different weight percentages (1, 3, 5 and 7) of Sn Ag Cu powder into an eutectic Sn 9Zn solder paste. The influence of a small amount of Sn Ag Cu powder on the microstructural evolution, especially, the morphology and distribution of intermetallic compound (IMC) particles were investigated on ball grid array (BGA) substrates using metallographic analysis. In addition, the shear strengths of the Sn Zn solder and Sn Ag Cu content solders on the ball grid array (BGA) packages were measured depending on the number of reflow cycles and content of reinforcing Sn Ag Cu. 2. Experimental procedure To prepare 0.76 mm diameter solder balls, Sn 9Zn (Showa Denko JUFFIT-E 9ZSN10 M) solder paste was taken from the refrigerator and kept it for one hour at a room temperature (21 C) and then mixed with different weight percentages of Sn 3.5Ag 0.5Cu powder (1, 3, 5 and 7). The mixture was blended manually for at least 30 min to ensure uniform distribution of the Sn 3.5Ag 0.5Cu particles. Then, the paste mixtures were printed on alumina substrates using a stainless steel stencil with a thickness of 0.15 mm and reflowed in a reflow oven (BTU VIP-70N) at 245 C. A solder mask-defined copper bond pad on the flexible substrate of a BGA package was used as a base for the electrodeposition of Ni and Au. The solder mask-opening diameter was 0.6 mm with a 7 lm thick Ni layer on the ball pad. The average thickness of the Au layer was 0.5 lm. Lead-free solder balls with a diameter of 0.76 mm, were placed on prefluxed Au/Ni/Cu bond pads of the substrates as shown in Fig. 1 and reflowed at a temperature of 245 C with a belt speed 10 cm/min in a convection reflow oven (BTU VIP-70 N). Fig. 1. Schematic diagram of a solder ball attachment on a flexible substrate. To characterize the microstructures, the reflowed samples were cross sectioned and mounted in resin, then ground by different grit sizes of emery papers and polished with 0.5 lm Al 2 O 3 powder. Finally, the interfacial morphology at the solder alloy/bga substrate interface was observed using a scanning electron microscope (SEM, Philips XL 40 FEG) with the backscattered electron (BSE) imaging mode and an energy dispersive X-ray spectrometer (EDAX International, model no. DX-4) was utilized for determining the chemical composition of the intermettalic compound (IMC) particles. The accuracy of the compositional measurements was typically ±5%. To find out the formula composition of the intermetallic compound (IMC) particles, the chemical analyses of the EDX spectra were corrected by standard atomic number, absorption, fluorescence (ZAF) software. Before SEM observations, the samples were sputter coated with Au to avoid effects due to charging. To measure the shear strength, ball shear tests were performed on reflowed samples using a shear testing machine (PTR-1000, Rhesca Co. Ltd., Japan) with a 100 lm shear tool height and a 550 lm/s shear speed. The average strength of twenty solder joints with the minimum and maximum values removed was taken for Fig. 2. SEM micrographs of (a) Sn Zn, (b) Sn Zn/1 wt% Sn Ag Cu, (c) Sn Zn/3 wt% Sn Ag Cu and (d) Sn Zn/7 wt% Sn Ag Cu solder joints after one reflow cycle.
3 A.K. Gain et al. / Microelectronic Engineering 86 (2009) Fig. 3. SEM micrographs of (a) Sn Zn, (b) Sn Zn/1 wt% Sn Ag Cu, (c) Sn Zn/3 wt% Sn Ag Cu and (d) Sn Zn/7 wt% Sn Ag Cu solder joints after one reflow cycle. The arrowheads in (a) point to acicular-shaped Zn-rich phase whilst in (b d) the arrowheads point to e-agzn 3 intermetallic compound particles. each condition. After ball shear testing, the fracture surfaces and composition were investigated thoroughly using SEM and EDX. 3. Results and discussion Fig. 2 shows cross-sectioned backscattered electron micrographs of interfaces between (a) Sn Zn, (b) Sn Zn/1 wt% Sn Ag Cu, (c) Sn Zn/3 wt% Sn Ag Cu, (d) Sn Zn/7 wt% Sn Ag Cu solders and Au/Ni/Cu BGA substrates after one reflow cycle. It is generally known that Au dissolves into the solder matrix quickly, after which Ni 3 Sn 4 IMC particles are formed at the interface during reflow with Sn Pb and Sn Ag solders [17]. From the backscattered electron micrographs shown in Fig. 2a, the scallop-shaped AuZn 3 intermetallic compound in light contrast was clearly observed at the interfaces due to the fast reaction between Zn and Au. On the other hand, after the addition of different weight percentages of the Sn Ag Cu, the interfacial microstructures were significantly changed as shown in Fig. 2b d. In the Sn Ag Cu content solders, an additional e-agzn 3 intermetallic compound layer in dark contrast was found to adhere on the top surface of the AuZn 3 intermetallic compound layer. In addition, after the addition of the Sn Ag Cu, fine spherical-shaped e-agzn 3 intermetallic compound particles were clearly observed as indicated with arrow heads in Fig. 2c and d which were adhered on the e-agzn 3 layer. However, with an increase in the Sn Ag Cu content, the amount of fine spherical-shaped e-agzn 3 intermetallic compound particles increased as shown in Fig. 2b d. In the plain Sn Zn solder, some microvoids were found at interfaces as indicated with arrowheads in Fig. 2a. However, after the addition of the Sn Ag Cu, no defects were found at their interfaces. Fig. 3 shows backscattered electron micrographs of (a) Sn Zn, (b) Sn Zn/1 wt% Sn Ag Cu, (c) Sn Zn/3 wt% Sn Ag Cu and (d) Sn Zn/7 wt% Sn Ag Cu solders which were taken from solder ball regions after one reflow cycle. The fine acicular-shaped Zn-rich phase in dark contrast as indicated with arrowheads in Fig. 3a was clearly observed in the gray color b-sn matrix in the Sn Zn solder joint. It is known that the solid solubility of Sn in Zn is less than 0.05 wt% and the maximum solid solubility of Zn in Sn is approximately 2 wt% [18]. However, after the addition of the Sn Ag Cu, fine spherical-shaped e-agzn 3 intermetallic compound particles as indicated with arrowheads in Fig. 3b d were detected as well as the acicular-shaped Zn-rich phase in the b-sn matrix. The amount of e-agzn 3 intermetallic compound particles increased as the Sn Ag Cu content increased. Song et al. [19] reported that Ag reacts with Sn Zn solder and results in the formation of primary intermetallic dendrites b-sn Ag Zn and c-agzn 8 inside and e- AgZn 3 in the outer peripheral regions. Fig. 4 shows cross-sectioned backscattered electron micrographs of interfaces between (a) Sn Zn/1 wt% Sn Ag Cu, (b) Sn Zn/3 wt% Sn Ag Cu, (c) Sn Zn/5 wt% Sn Ag Cu, (d) Sn Zn/7 wt% Sn Ag Cu solders and Au/Ni/Cu BGA substrates after four reflow cycles. After four reflow cycles, their interfacial microstructures were not significantly changed. However, the e-agzn 3 intermetallic compound layer thickness as well as adhere spherical-shaped e- AgZn 3 intermetallic compound as indicated with arrowheads in Fig. 4b d size increased with an increase in the number of reflow cycles. Fig. 5 shows the cross-sectioned backscattered electron micrographs of interfaces between (a) Sn Zn/1 wt% Sn Ag Cu, (b) Sn Zn/3 wt% Sn Ag Cu, (c) Sn Zn/5 wt% Sn Ag Cu (d) Sn Zn/7 wt% Sn Ag Cu solders and Au/Ni/Cu BGA substrates after eight reflow cycles. From Figs. 2, 4 and 5, it is clear with an increase in the number of reflow cycles, the e-agzn 3 layer thickness increased due to an increase in the reaction time between the Ag rich and the Zn rich phases. In general, with an increase in the number of reflow cycles as well as reflow time the scallop-shaped AuZn 3 phase floated and moved away from the interfaces [20]. However, in the present study, it was confirmed that with an increase in the number of reflow cycles the scallop-shaped AuZn 3 layer as well as the e-agzn 3 layer were well adhered at the interfaces. Fig. 6 shows the cross-sectioned backscattered electron micrographs of (a) 1 wt%, (b) 3 wt%, (c) 5 wt% and (d) 7 wt% Sn Ag Cu content solders which were taken from solder ball regions after eight reflow cycles. A mixture of the acicular-type Zn-rich phase, the spherical-shaped e-agzn 3 intermetallic compound particles and the b-sn phase were clearly observed the same as in Fig. 3. However, with an increase in the number of reflow cycles, the spherical-shaped e-agzn 3 intermetallic compound size has
4 2350 A.K. Gain et al. / Microelectronic Engineering 86 (2009) Fig. 4. SEM micrographs of (a) Sn Zn/1 wt% Sn Ag Cu Sn Zn, (b) Sn Zn/3 wt% Sn Ag Cu, (c) Sn Zn/5 wt% Sn Ag Cu and (d) Sn Zn/7 wt% Sn Ag Cu solder joints after four reflow cycles. The arrowheads in (a d) again point to e-agzn 3 intermetallic compound particles. Fig. 5. SEM micrographs of (a) Sn Zn/1 wt% Sn Ag Cu, (b) Sn Zn/3 wt% Sn Ag Cu, (c) Sn Zn/5 wt% Sn Ag Cu and (d) Sn Zn/7 wt% Sn Ag Cu solder joints after eight reflow cycles. The arrowheads in (a d) again point to e-agzn 3 intermetallic compound particles. increased. From a reliability test, Jiang et al. [21] reported that after exposing Sn Zn solder to 85 C/43%RH (relative humidity) and 85 C/85%RH atmospheres, the oxidation of Sn Zn solder is attributed to the oxidation of Zn, which diffuses to the Sn grain boundaries and forms ZnO. These oxides are liable to give rise to cracks along the Sn grain boundaries. In our present study, the formation of spherical-shaped e-agzn 3 intermetallic compound can improve the oxidation resistance of the Sn Zn solder. During soldering, these intermetallic compounds will form in the grain boundaries and later on block the penetration of the water vapor and oxygen which in turn reduces the formation of ZnO along the grain boundaries. Since solder joints are often subjected to mechanical loading during processing and system use, the mechanical properties of solder joints such as shear strength and creep resistance, are important for their reliability. Therefore, ball shear tests were performed to evaluate the properties of the solder joints as a function of the number of reflow cycles as well as the Sn Ag Cu content and the results are represented in Fig. 7. In case of the Sn Zn solder, the shear load was about 1.80 kg. However, in the Sn Ag Cu content solders, the shear loads increased with an increase in the Sn Ag Cu content for each investigated number of reflow cycles due to uniform distribution of e-agzn 3 intermetallic compound (IMC) particles. The shear loads of 1 wt%,
5 A.K. Gain et al. / Microelectronic Engineering 86 (2009) Fig. 6. SEM micrographs of (a) Sn Zn/1 wt% Sn Ag Cu, (b) Sn Zn/3 wt% Sn Ag Cu, (c) Sn Zn/5 wt% Sn Ag Cu and (d) Sn Zn/7 wt% Sn Ag Cu solder joints after eight reflow cycles. The arrowheads in (a d) point to e-agzn 3 intermetallic compound particles. Fig. 7. Shear loads of Sn Zn solder and Sn Ag Cu content solder joints depending on the number of reflow cycles. 3 wt% 5 wt% and 7 wt% Sn Ag Cu content solder joints after one reflow cycle were about 1.90, 1.92, 1.95 and 2.03 kg and their shear loads after eight reflow cycles were about 1.78, 1.80, 1.85 and 1.88 kg. The detailed fracture behavior of Sn Zn solder and the Sn Ag Cu content solders may be revealed by extensive fractrographic observations. SEM micrographs of fracture surfaces at lower magnification with the various additions of Sn Ag Cu can be seen in Fig. 8b d having (b) 1 wt%, (c) 5 wt% and (d) 7 wt% Sn Ag Cu content. Fig. 8a shows the fractograph of Sn Zn solder. The fracture surface of the Sn Zn solder exhibited a brittle fracture mode with a smooth surface. On the other hand, the Sn Ag Cu content solders showed ductile failure with very rough dimpled surfaces as shown in Fig. 8b d. In the Sn Ag Cu content solders, some dimples were clearly observed in the fracture surfaces as indicated with arrow heads in Fig. 8b d due to the formation of fine e-agzn 3 intermetallic compound particles. Micrographs of fracture surfaces with different additions of Sn Ag Cu are given after eight reflow cycles in Fig. 9. Fig. 9a and b are the fractographs of 3 wt% Sn Ag Cu content sample, while in Fig. 9c and d are 7 wt% Sn Ag Cu content sample. From these SEM micrographs it is clear that the fracture mode is ductile with the characteristic rough dimpled surfaces. However, the dimple size increased with an increase in the number of reflow cycles due to the increase in the size of the e-agzn 3 intermetallic compound particles.
6 2352 A.K. Gain et al. / Microelectronic Engineering 86 (2009) Fig. 8. SEM fracture surfaces of (a) Sn Zn, (b) Sn Zn/1 wt% Sn Ag Cu, (c) Sn Zn/5 wt% Sn Ag Cu and (d) Sn Zn/7 wt% Sn Ag Cu solder joints after one reflow cycle. Fig. 9. SEM fracture surfaces of (a, b) Sn Zn/3 wt% Sn Ag Cu and (c, d) Sn Zn/7 wt% Sn Ag Cu solder joints after eight reflow cycles. 4. Conclusions Small amounts of Sn Ag Cu powder were added into a Sn Zn eutectic solder to investigate the impacts of Sn Ag Cu additions on the formation, growth and evolution of the IMC layer structure at the Au/Ni/Cu BGA substrate/solder interfaces. In the plain Sn Zn solder, scallop-shaped AuZn 3 intermetallic compound was found at the interfaces. However, in the Sn Ag Cu content solders, an additional e-agzn 3 intermetallic compound layer was found to be well adhered on the top surface of the AuZn 3 layer and its thickness increased when the number of reflow cycles increased. In addition, fine spherical-shaped e-agzn 3 intermetallic compound particles and an acicular-shaped Zn-rich phase was clearly observed in the b-sn matrix. With an increase in the Sn Ag Cu content, the number of fine spherical-shaped e-agzn 3 intermetallic compound particles increased and their size increased when the number of reflow cycles increased. In the Sn Ag Cu content solders, the fracture surfaces exhibited typical ductile behavior with very rough dimpled surfaces. The shear load increased with an increase in the Sn Ag Cu content due to the uniform distribution of e-agzn 3 intermetallic compound (IMC) particles. Their shear loads after one reflow cycle were increased from 1.80 to 2.03 kg and after eight reflow cycles their shear loads were increased from 1.67 to 1.88 kg.
7 A.K. Gain et al. / Microelectronic Engineering 86 (2009) Acknowledgements The authors acknowledge the financial support provided by City University of Hong Kong for the project CERG grant of Hong Kong Research Grants Council and RGC Ref. No (Development of a nano-activator doped surface modifier for Sn Zn based lead-free soldering). Professor Brian Ralph is thanked for proof reading the manuscript. References [1] W.H. Zhong, Y.C. Chan, M.O. Alam, B.Y. Wu, J.F. Guan, J. Alloy. Compd. 414 (2006) [2] R.A. Islam, B.Y. Wu, M.O. Alam, Y.C. Chan, W. Jillek, J. Alloy. Compd. 392 (2005) [3] Y.W. Lee, K.J. Lee, Y.N. Zhou, J.P. Jung, Microelectron. Reliab. 48 (2008) [4] X.F. Zhang, J.D. Guo, J.K. Shang, Scripta Mater. 57 (2007) [5] S. Vaynman, M.E. Fine, Scripta Mater. 41 (12) (1999) [6] T. Ichitsubo, E. Matsubara, K. Fujiwara, M. Yamaguchi, H. Irie, S. Kumamoto, T. Anada, J. Alloy. Compd. 392 (2005) [7] P.C. Shih, K.L. Lin, J. Alloy. Compd. 439 (2007) [8] K.K. Mohan, V. Kripesh, L. Shen, K. Zeng, A.A.O. Tay, Mater. Sci. Eng. A 423 (2006) [9] M.N. Islam, Y.C. Chan, M.J. Rizvi, W. Jillek, J. Alloy. Compd. 400 (2005) [10] C.Y. Chou, S.W. Chen, Acta Mater. 54 (2006) [11] J.E. Lee, K.S. Kim, M. Inoue, J. Jiang, K. Suganuma, J. Alloy. Compd. 454 (2008) [12] P. Yao, P. Liu, J. Liu, J. Alloy. Compd. 462 (2008) [13] K.K. Mohan, V. Kripesh, A.A.O. Tay, J. Alloy Compd. 455 (2008) [14] M. McCormack, H.S. Chen, G.W. Kammlott, S. Jin, J. Electron. Mater. 26 (8) (1997) [15] A. Fawzy, Mater. Charact. 58 (2007) [16] F. Guo, J. Lee, S. Choi, J.P. Lucas, T.R. Bieler, J. Electron. Mater. 30 (2001) [17] M.N. Islam, Y.C. Chan, A. Sharif, J. Mater. Res. 19 (2004) [18] J.W. Yoon, S.B. Jung, Mater. Sci. Eng. A (2007) [19] J.M. Song, K.L. Lin, J. Mater. Res. 19 (9) (2004) [20] S.C. Chang, S.C. Lin, K.C. Hsieh, J. Alloy. Compd. 428 (2007) [21] J. Jiang, J.E. Lee, K.S. Kim, K. Suganuma, J. Alloy. Compd. 462 (2008)
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