THE EFFECTS OF Bi AND AGING ON THE MICROSTRUCTURE AND MECHANICAL PROPERTIES OF Sn-RICH ALLOYS

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1 THE EFFECTS OF Bi AND AGING ON THE MICROSTRUCTURE AND MECHANICAL PROPERTIES OF Sn-RICH ALLOYS André Delhaise and Doug Perovic University of Toronto Toronto, ON, Canada Polina Snugovsky, Ph.D. Celestica, Inc. Toronto, ON, Canada ABSTRACT This paper examines the effects of Bi on the microstructure and hardness of Sn-Bi and Sn-Cu-Bi alloys subjected to ageing treatments at room and elevated temperatures. One main concern with SAC alloys that has led to research of Bi-containing alloys is the degradation of mechanical and thermomechanical properties due to the coarsening of microstructure during aging, and in earlier studies, the inclusion of Bi in the alloy results in a uniformity of microstructure and an increase in alloy hardness. The goal of this paper and ongoing research is to investigate whether these trends hold for binary alloys, and to understand what mechanisms are responsible for these effects. Four alloys Sn-1Bi, Sn-5Bi, Sn-0.7Cu-1Bi, and Sn- 0.7Cu-5Bi - were aged at room temperature for 10 days or 28 days. Two of these, Sn-1Bi and Sn-5Bi, were aged at 100 o C for 7 days, and were all cooled in air. The microstructure of the samples after solidification and aging were compared using Scanning Electron Microscopy (SEM). Alloy hardness after solidification and aging was measured using a Rockwell hardness tester HR15X with a ¼ Carbide ball indenter. In alloys containing Bi precipitates, these particles became more uniformly distributed with aging. Hardness was observed to not undergo any significant changes after aging, which differs significantly from SAC alloys. Keywords: Bismuth, Aging, Microstructure, Hardness INTRODUCTION With the phasing out of lead-containing alloys in the electronics manufacturing industry as a result of legislation such as the Restriction of Hazardous Substances (RoHS), lead-free solders such as SAC305 (Sn-3.0Ag-0.5Cu) have become the principal joining materials in electronic devices. The main concern with lead is toxicity and while this issue is addressed by utilizing lead-free solders instead, several new problems arise. As a result, SAC alloys are less wellsuited as replacements, and has led to the continuing development of new lead-free alloys: Melting temperature SAC alloys have a significantly higher melting point. This has led to the need for use of high T g board materials, which are more susceptible to failure modes such as pad cratering. Cost With the removal of lead and the addition of silver, material cost increases. With a higher melting temperature, the cost of manufacturing processes increases. Whiskers Pb tends to suppress whisker formation; with the removal of lead, whiskers can grow to lengths that may cause short circuit failures. Reduced reliability Silver and copper tends to form intermetallic compounds (IMCs) with Sn such as Ag 3 Sn and Cu 6 Sn 5 these reduce the toughness of the alloy and subsequently performance in accelerated reliability tests such as drop and thermal cycling. Degradation of Microstructure during aging Numerous studies 1,2,3,4 have shown that the microstructure of SAC coarsens and recrystallizes over time (Figure 1), which leads to a decay in mechanical properties (Figure 2). These concerns have led to an increased interest in developing new lead-free solder alloys which remedy the above issues. Bismuth (Bi) has shown to be a promising alloying element the Sn-Bi binary phase diagram (Figure 3) indicates that Bi should reduce the melting point, which would decrease manufacturing costs, allow for the use of standard T g board materials and reduce the likelihood of thermal damage to assemblies. Furthermore, the phase diagram suggests

2 that Bi does not form any IMCs with Sn these phases tend to be brittle and can reduce reliability. Rather, Bi will exist in solid solution with tin (fully dissolved) and possibly, depending on Bi content and temperature, also as a secondary precipitate phase with the tin matrix. It is therefore likely that solid-solution strengthening and precipitation hardening by this secondary Bi phase increase the strength of the alloy. Bi has also been shown in some preliminary studies to inhibit the growth of tin whiskers in a similar mechanism as Pb 6. Figure 2: Evolution in mechanical properties of SAC305 after aging. Hardness after aging at 100C 3 (top); Ultimate tensile strength after room temperature aging 3 (bottom). Figure 1: Evolution of Microstructure of SAC305, after aging at 125C 1 Several studies have investigated the effects of bismuth on the microstructure and mechanical properties of aged lead-free alloys 1,7,8,9,10,11. In all of these studies, it was shown that Bi-containing alloys are more resistant to mechanical degradation caused by aging. In one joint UofT/Celestica study in , seven Bi-containing alloys were subjected to aging at 100 o C for either 25 hours or 100 hours. The microstructure of these alloys underwent substantial changes deviating from a typical dendritic as-cast microstructure with IMCs and Bi situated in the interdendritic regions, to a more uniform microstructure with these secondary phases distributed equally throughout (Figure 4). This corresponded to a marked increase in alloy hardness Figure 3: Sn-Bi phase diagram 5.

3 (Figure 5), indicating that Bi could potentially be used to age- harden Pb-free solder alloys. These dendritic as-cast This study is associated with the Refined Manufacturing Acceleration Process (ReMAP) Materials research area, specifically the M3 Aging project. It follows a similar methodology to this past UofT/Celestica study, however the main alloy system under investigation is the binary Sn-Bi system. The effects of aging on alloy microstructure and hardness are examined in this study. EXPERIMENTAL APPROACH Alloys The binary Sn-Bi system is the primary family of alloys under consideration in this study. This is considerably different from the main ReMAP M3 project, which focuses on more practical alloys (Cu and Ag additions improve wetting properties, for example). Selecting the binary system allows for direct analysis of the effects of Bi on the properties of the alloy, without any potentially influential effects by alloying elements such as Cu and/or Ag. Bi content was chosen to be similar to the more practical alloys under consideration by the main M3 ReMAP project (less than 7wt%). Higher Bi content has been shown to have a negligible influence on alloy properties, and may produce an undesirable microstructure. For example, at high Bi content, the encapsulation of Sn grains by Bi precipitates severely weakens grain boundaries (Figure 6). The alloys considered in this study to this point contain 1, 3, 5, or 7 wt% Bi. Figure 4: Evolution of the microstructure of "Orchid" (Sn-2.0Ag-7.0Bi) after aging at 100C for 300h 10. As cast microstructure (top); aged microstructure (bottom). Figure 6: Sn-10Bi aged at 100C for 3 days, showing distribution of Bi at grain boundaries. Figure 5: Evolution of Hardness of Bi-containing alloys after aging at 100C 10. Cu-containing alloys are also being studied to examine the effects of a second alloying element on microstructure and mechanical properties. The family of alloys chosen is the Sn-Cu-Bi system, where Cu content is kept constant at 0.7wt% and Bi content is varied. Bi content was chosen to directly correlate with the selected compositions for Sn-Bi 1, 3, 5, or 7wt% Bi.

4 Sample Preparation Samples were roughly 10g in size to allow for a uniform temperature gradient during the aging process. These were prepared using two master alloys one containing 7wt% Bi, the other containing no Bi. Pieces of each were weighed to yield the desired compositions, and were melted in an alumina crucible on a laboratory hot plate. These were then cooled for seven minutes on an iron slab at room temperature. For each alloy/aging condition, 4 samples were prepared two for microstructure analysis, the other two for hardness testing. Aging Profiles Alloys were left in either as-cast conditions, or subjected to aging at room temperature or elevated temperature. Room temperature aging involves leaving the alloys in the laboratory at room temperature (roughly 22 o C). In this paper, only results from 10 and 28 days are shown. Elevated temperature aging was conducted at 100 o C for 7 days. moisture after the final polish. Samples prepared in this manner were free of moisture during SEM analysis. This step is especially important for as-cast microstructure. The samples were then analyzed using SEM (Hitachi SU-3500). Hardness Sample surfaces required for hardness testing were prepared using the two coarsest grinding papers only. Samples then underwent Rockwell hardness testing using a 1/4 carbide ball indenter (superficial, 15X scale). 9 readings were taken from each sample the highest and lowest measurements on each sample were excluded, and the remaining measurements were averaged. Figure 7 shows an image of a typical indentation using this testing method. Table 1 below gives a breakdown of the results shown in this paper for each alloy. The main alloys being considered are Sn-1Bi, Sn-5Bi, Sn-0.7Cu-1Bi, and Sn- 0.7Cu-5Bi; the as-cast hardness for the remaining alloys was included to provide a fuller representation of how Bi content affects hardness. Table 1: Summary of Analyses on Alloys Alloy Microstructure Hardness Sn No As cast only Sn-1Bi All All Sn-3Bi No As cast only Sn-5Bi All All Sn-7Bi No As cast only Sn-0.7Cu No As cast only Sn-0.7Cu-1Bi As cast, Room As cast, Room Temperature Temperature Sn-0.7Cu-3Bi No As cast only Sn-0.7Cu-5Bi As cast, Room Temperature Sn-0.7Cu-7Bi No As cast only As cast, Room Temperature Microstructure To prepare the samples for Scanning Electron Microscopy (SEM), a series of progressively finer silicon carbide (SiC) papers and 6µm diamond paste were used. Final polishing was done using colloidal silica. To ensure the observed microstructure was truly representative of the bulk alloy microstructure, sample preparation was done immediately preceding SEM inspection. Samples were placed in vacuum for at least twenty minutes in order to draw out all residual Figure 7: Indentation of 1/4" ball on Sn-0.7Cu-1Bi sample. RESULTS As-cast As-cast microstructure was analyzed for Sn-1Bi and Sn-5Bi, as well as their copper-containing counterparts (Figure 8). As the solid solubility of Bi in Sn at room temperature is roughly 2wt%, Bi for the most part is not visible in the Sn-1Bi and Sn-0.7Cu-1Bi alloys, however small clusters are observable in places. More Bi precipitates are observable in the copper-containing alloy, as the presence of copper reduces the solid solubility of Bi in Sn. The copper-containing alloy also contains numerous Cu 6 Sn 5 intermetallics. These are also located in the interdendritic spaces as they form from the last remaining liquid. The samples containing 5wt% Bi predictably show significantly more precipitation of Bi. Bi tends to form in large clusters and the microstructure in general is quite non-uniform.

5 Hardness testing of the as-cast alloys revealed that increasing bismuth content increases hardness, for both the binary and ternary alloys (Figure 9), and that solidsolution strengthening and precipitation hardening are the likely mechanisms behind these changes. In close agreement with a previous study 9, it was seen that at around 5wt% Bi, hardness starts to plateau, indicating that optimal reliability can be achieved with bismuth content at or around this level. Copper has a significantly larger effect on alloy hardness at lower Bi content at higher Bi content the copper containing alloy has nearly identical hardness as the corresponding binary alloy. Pure Sn could not be measured using this hardness scale as it was too soft. Figure 9: As-cast hardness for Sn-xBi and Sn-0.7CuxBi alloys. Room Temperature The four alloys investigated after room temperature aging did not demonstrate any appreciable changes in microstructure after both 10 and 28 days of aging, with the exception of the Sn-5Bi alloy (Figure 10). The Sn-1Bi alloy microstructure remained nearly identical owing to the single phase present. In the Sn- 0.7Cu-1Bi alloy, intermetallic particle size did not change significantly, and the overall microstructure indicates that the dendritic structure of tin remained intact after aging. In the alloys containing 5% Bi, Bi precipitates remained clustered, however these clusters grew larger and precipitates became more variable in size. These changes were more significant for the binary alloy. The hardness of the four alloys investigated did not change considerably with aging time at room temperature (Figure 11). This is a distinctly different result that what was observed for SAC 3, in which a pronounced decay in strength was observed after just five days. Figure 8 (opposite): From top to bottom, as-cast microstructure of Sn-1Bi, Sn-0.7Cu-1Bi, Sn-5Bi,, and Sn-0.7Cu-5Bi.

6 Figure 11: Hardness of select Sn-xBi and Sn-0.7CuxBi alloys after room temperature aging. High Temperature Only two alloys were aged at 100 o C to this point in the study Sn-1Bi and Sn-5Bi. The microstructure of the former remained largely the same as the as-cast after aging. In the latter, the microstructure changed significantly the Bi particles became more uniformly distributed throughout the microstructure (Figure 12). The solvus temperature (at which all precipitates fully dissolve into the matrix upon heating) of Sn-5Bi is approximately 60 o C. Therefore, heating the sample to 100 o C allows for all Bi to enter solid solution. In addition, as diffusion occurs more rapidly at higher temperatures, Bi can distribute itself more equally throughout the matrix, and precipitation is more uniform upon cooling to room temperature. In the 1Bi alloy, aging at a high temperature ensured all precipitates fully dissolved in the Sn matrix, and hence no Bi precipitates were visible, unlike in the as-cast and room temperature-aged samples. Alloy hardness does not change considerably with time at 100 o C (Figure 13). This is comparable to several earlier studies 1,7,10, which showed that the strength of bismuth-containing alloys is more stable after hightemperature ageing. DISCUSSION It was seen that the addition of copper to the alloy has a larger effect on hardness when Bi content is low, and has very little effect at higher (~5wt%) levels of Bi in the alloy. This is likely the result of competing mechanisms of Bi solid solution strengthening, Bi precipitation, and Cu 6 Sn 5 IMCs. The reason precipitates were visible in the as-cast Sn- 1Bi alloy, despite the phase diagram indicating otherwise, is because the phase diagram assumes a very slow cooling Figure 10 (opposite): From top to bottom, microstructure after room temperature aging: Sn- 5Bi after 10d and 28d, Sn-0.7Cu-5Bi after 10d and 28d.

7 rate far slower than what occurs in reality. As a result, as Sn solidifies in dendrites, the interdendritic material (last remaining liquid) can become supersaturated with Bi. As the last of the liquid solidifies, Bi can be forced out of solid solution into precipitate form if the local Bi content is high enough. It was observed that the hardness of these Bi-containing alloys does not behave in the same manner as that of SAC after aging. This is in agreement with earlier studies 1,7,10, which show that hardness is not degraded. It is therefore evident that Bi, in precipitate and/or solid solution form, contributes to the stabilization of properties. Figure 12: Microstructure after aging at 100C for 7d. Sn-1Bi (top); Sn-5Bi (bottom). Figure 13: Hardness of select Sn-xBi alloys after aging at 100C. The dendritic tin structure, as well as IMC distribution and size, did not undergo any noticeable changes after aging. The only aspect of the microstructure that showed any observable changes were the bismuth precipitates in the alloys containing 5wt% Bi. The clusters in general tended to grow larger and average precipitate size decreased. In the samples aged at elevated temperature, the Bi precipitates also spread more evenly throughout the microstructure, due to accelerated diffusion at higher temperature, and that all Bi entered solid solution during the aging process. The likely reason the microstructure did not become fully uniform is because not enough time had elapsed. Longer elevated temperature aging tests will be performed to determine this. Elevated temperature tests will also be performed on copper-containing alloys to discern whether the Sn or IMCs undergo change in these conditions. CONCLUSIONS Several Sn-Bi and Sn-0.7Cu-Bi alloys were subjected to aging at either 100 o C for 7 days, or at room temperature for 10d or 28d. The as-cast microstructure was made up of Sn dendrites with dissolved Bi, and depending on the Bi/Cu content, clusters of Bi precipitates and Cu 6 Sn 5 intermetallics situated in the interdendritic regions. For both alloy systems, hardness was seen to increase with Bi content (likely as a result of solid-solution strengthening and precipitation hardening) up to approximately 5wt% Bi, after which it plateaus. When the same amount of copper is added to alloys with varying Bi content, the copper increases hardness to a greater extent at low Bi content, and the coppercontaining alloy has nearly identical hardness as the binary alloy at higher Bi content. This is believed to be the result of the strengthening effects of Bi and Cu 6 Sn 5 competing with one another. Aging the alloys at room temperature caused few changes in the dendritic structure of the Sn or size and distribution of the IMCs, however the Bi precipitate

8 clusters in general tended to grow larger and precipitates became finer. This was especially noticeable in the Sn-5Bi alloy. Aging at 100 o C did not result in any observable changes to the microstructure of Sn-1Bi, however the microstructure of Sn-5Bi became noticeably more uniform. Hardness was not significantly changed with these aging treatments, a significant difference from SAC alloys. This confirmed results from earlier papers which showed a stabilization of the mechanical properties of Bi-containing alloys after aging. FUTURE WORK The results in this paper only show two time points for room temperature aging, however aging times up to six months will be examined in future, up to six months. It is hoped that these results will give a clearer indication of the effects of room temperature aging for Sn-Bi and Sn-Cu-Bi alloys. Further elevated temperature aging experiments are planned, involving more alloys, time points and temperatures. Temperatures will be selected based on the solvus temperature of each alloy selected. Aging above the solvus yields similar microstructures to those shown in this paper very uniform due to the dissolution of Bi and evenly distributed precipitates upon cooling. Aging below the solvus leads to particle coarsening through a mechanism known as Ostwald ripening. Smaller particles tend to dissolve and diffuse towards the larger particles leading to a non-uniform particle size upon cooling. It is anticipated that very different properties will be observed when comparing alloys aged above and below the solvus. While it is fairly straightforward to determine what the effects of aging are on the microstructure and mechanical properties of these alloys, it is another challenge altogether to characterize the mechanisms behind these changes. Transmission Electron Microscopy (TEM) is a technique which will allow for examination of these alloys at very high resolutions and visualize these mechanisms for example Bi in solid solution will impart strain on the Sn lattice, which can be observed using strain mapping in the TEM. Finally, while hardness is a quick, easy method to gauge a material s strength, it does not give a complete picture of deformation and failure mechanisms. More advanced mechanical testing methods such as nanoindentation (to determine creep properties, similar to an earlier study 12 ), impact testing (to gauge toughness) and fatigue will be considered. ACKNOWLEDGMENTS The authors would like to thank the Department of Materials Science & Engineering at the University of Toronto, as well as ReMAP, for funding. REFERENCES 1 David Witkin, Mechanical Properties of Bicontaining Pb-Free Solders, APEX Expo 2013, San Diego, CA, February 16-21, H. Ma, J. Suhling, et al., The Influence of Elevated Temperature Aging on Reliability of Lead Free Solder Joints, 2007 Electronic Components and Technology Conference, John Ascuaga s Nugget Sparks, NV, USA, May 29-Jun 1, M. Hasnine, M. Mustafa, J.C. Suhling et al., Characterization of Aging Effects in Lead Free Solder Joints Using Nanoindentation, 2013 Electronic Components and Technology Conference, Las Vegas, NV, USA, May 29-31, H. Ma, J. Suhling, et al., Reliability of the Aging Lead-free Solder Joint, 2006 Electronic Components and Technology Conference, San Diego, CA, May 30- June 2, National Institute of Standards and Technology (NIST), Phase Diagrams and Computational Thermodynamics Bi-Sn System, [Online]. Available: 6 N. Jadhav et al., Altering the Mechanical Properties of Sn Films by Alloying with Bi: Mimicking the Effect of Pb to Suppress Whiskers, Journal of Electronic Materials, 42, 2 (2013), pp P. Snugovsky et al., Reliability Screening of Lower Melting Point Pb-Free Alloys Containing Bi, APEX Expo 2014, Las Vegas, NV, March 25-27, P. Vianco, et al., Properties of Ternary Sn-Ag-Bi Solder Alloys: Part 1- Thermal Properties and Microstructural Analysis, J. Electronic Materials, 28, 10 (1999), pp P. Vianco, et al., Properties of Ternary Sn-Ag-Bi Solder Alloys: Part 2- Wettability and Mechanical Properties Analysis,, J. Electronic Materials, 28, 10 (1999), pp A. Delhaise et al., Microstructure and Hardness of Bi-containing Solder Alloys after Solidification and Ageing, J. Surface Mount Technology, 27, 3 (2014), pp D. Witkin, Creep Behavior of Bi-Containing Lead- Free Solder Alloys, Journal of Electronic Materials, 41, 2 (2012), pp

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