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Effect of Composition and Cooling Rate on the Microstructure of SnAgCu-Solder

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Conference Paper in Proceedings - Electronic Components and Technology Conference · July 2007
DOI: 10.1109/ECTC.2007.374006 · Source: IEEE Xplore

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 Effect of Composition and Cooling Rate on the Microstructure of SnAgCu-Solder Joints

M. Mueller, S. Wiese, M. Roellig and K.-J.Wolter

Technische Universität Dresden, IAVT
D-01062 Dresden, Germany
maik.mueller@avt.et.tu-dresden.de, +49 351 463 33172

varied from bulk specimen to solder balls of different sizes,

Abstract
which are comparable with BGA, CSP and flip chip
In this study the solder alloys SnAg3.5, SnAg3.0Cu0.5,
interconnects. This comparison is necessary to understand
SnAg3.8Cu0.7 and SnAg2.7Cu0.4Ni0.05 have been analysed
differences in material behaviour of different specimen sizes.
in order to determine variations in microstructure caused by
In addition the influences of cooling rate and solder
cooling rate, solder composition and ball diameter. Solder
composition were also investigated in order to find
spheres with a diameter of approx. Ø 1100 µm, Ø 590 µm,
correlations between these parameters. Furthermore, it will
Ø 270 µm and Ø 130 µm were solidified with cooling rates of
also be discussed how these factors influence the
0.14 K/s, 1.1 K/s and 10.9 K/s. Cross sections of these
solidification process.
specimens were analysed by optical light microscopy.
Interpretations of the analysed microstructure allow a
description of the solidification process, which takes place in
a solder ball. It could be concluded that this process is divided
in three stages: the formation of primary intermetallics, the
formation of fine structured regions and the formation of
coarse dendritic areas.
Introduction
During the last years an immense progress in developing
lead free solder alternatives has been achieved. Many studies
were carried out in order to investigate the material behaviour
and the microstructure of SnAgCu. Both properties are
directly connected with each other and show influences on
various factors, like reflow process conditions, alloy
composition, pad metallisation and thermo-mechanical stress
[1-4].
Another important aspect for solder alloy development is
the advance in packaging physical design. At the moment flip
chip assemblies with solder bumps having a diameter of
90 µm are already in use [5]. The International Technology
Roadmap for Semiconductors (ITRS) identified the decrease
of the I/O pitch down to 20 µm as a major technological
challenge for the next years. Contemporary concepts [6]
already realised solder caps with heights of 25 µm at a
diameter of 25 µm. The effect of miniaturisation on the
microstructure of SnAgCu interconnects is not fully
understood, yet.
Investigations in [7] point out that the undercooling
becomes larger with decreasing ball diameter. It is also found,
that the appearance of “interlaced” areas (small, randomly
orientated grains) appears more frequently in smaller solder
joints [7]. In a study about scaling effects in mechanical
behaviour [8], the creep properties of flip chip bumps, FBGA
interconnects and bulk specimen were compared. The results
indicate that material behaviour changes with size.
Both studies indicate that there are microstructural
differences caused by the larger undercooling. These
differences might be responsible for a change in material Figure 1: Overview of the microstructure of as cast SnAgCu
properties. solder ingots solidified in test tubes a) SnAg3.0Cu0.5
This study focuses on the influence of volume on the (cooling rate 0.0057 K/s) and b) SnAg3.8Cu0.7 (cooling rate
microstructure of lead free SnAgCu solders. The volume was 0.0083 K/s)

1-4244-0985-3/07/$25.00 ©2007 IEEE 1579 2007 Electronic Components and Technology Conference
Investigations on bulk solder ingots
An investigation on the solidification behaviour of
SnAgCu alloys was carried out on bulk solder ingots. Details
are described in [9]. Briefly, large bulk solder ingots have
been solidified in test tubes. The influence of cooling rate
(0.006 K/s to 0.6 K/s) and solder composition
(SnAg3.0Cu0.5, SnAg3.5Cu0.4, SnAg3.8Cu0.7,
SnAg3.0Cu1.5 and SnAg3.0Cu0.5Au0.14) on the as cast
microstructure was examined. The volume of the bulk solder
ingots is approx. 1E-06 m³ (Ø 7 mm; length approx. 23 mm).
Fig. 1 gives an overview of the microstructural variation
within a solder ingot and compares the microstructure of the
hypoeutectic SnAg3.0Cu0.5 solder versus the near eutectic
SnAg3.8Cu0.7 solder at slow cooling rates. Fig. 2 shows
characteristic details of the microstructure that were found in
the cross sections of the solder ingots. Fig. 2 is divided in
coarse structured (left column; Fig. 2a,c,e) and fine structured
areas (right column; Fig. 2b,d,f). Usually this very different
appearance of microstructure can be found at different
locations of the ingot. There are also intermediate types of
microstructure.
Figure 2: Typical microstructure of coarse (left column) and
fine (right column) structured areas found in bulk solder
ingots with different solder composition (SnAg3.0Cu0.5,
SnAg3.8Cu0.7 and SnAg3.0Cu1.5)
The microstructure of the hypoeutectic SnAg3.0Cu0.5 solder
(Fig. 1a) is dominated by β-Sn dendrites. Between the
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dendritic structures, intermetallics of different sizes and
shapes have been formed (Fig. 2c,d). Needle shaped
intermetallics with lengths up to 200 µm can be found in the
coarse areas (Fig. 2c). Fine structured regions between the
dendrites (Fig 3a) show small globular intermetallics (<2 µm).
Figure 3: a) Small precipitations with different shape formed
between β-Sn dendrites in the SnAg3.0Cu0.5 solder ingot
cooled with 0.16 K/s; b) Eutectic region with small
precipitations formed in the centre area of a SnAg3.8Cu0.7
solder ingot cooled with 0.59 K/s
The ingots of the near eutectic SnAg3.8Cu0.7 solder have
a very heterogeneous microstructure with much less β-Sn
dendrites (Fig. 1b). In the centre regions of the specimen
eutectic solidified solder can be found with very small
(<2 µm), disperse arranged, globular intermetallics (Fig. 2b,
Fig 3b). In the outer regions a coarse microstructure with
large Ag3Sn plates covered in β-Sn (Fig 2a) has been formed.
These plates reach lengths up to 2 mm and a thickness up to
15 µm. Smaller Ag3Sn needles and Cu6Sn5 intermetallics can
be found between those large structures (Fig. 2a).
Figure 4: Effect of cooling rate on the microstructure of
SnAg3.8Cu0.7 and SnAg3.0Cu0.5 bulk solder ingots
By increasing the Cu content to 1.5 wt.%, the presence of
primary solidified Cu6Sn5 intermetallics was observed
(Fig. 2e,f). These intermetallics are formed as hexagonal rods In order to get spherical joints with a defined cooling rate,
and are also covered in pure β-Sn (Fig. 2f). comparable to conditions during reflow, the test setup shown
Fig. 4 shows the microstructure of SnAg3.0Cu0.5 and in Fig. 9 was used. The preforms were fluxed (WS600 -
SnAg3.8Cu0.7 at different cooling rates. Faster cooling Alpha Metals) and placed in the holes of the ceramic. This
decreases the size of primary Ag3Sn intermetallics in the setup was placed on
SnAg3.8Cu0.7 solder. The dendritic growth of β-Sn is also the preheated heating
effected by cooling. At higher rates the spacing of β-Sn plate at 250 °C
decreases and the dendrites become longer and more directed (Fig. 9a). The
(Fig. 4). For both investigated alloys the eutectic regions temperatures of the
shown in Fig. 3 become larger with faster cooling. heater and the ceramic
Undercooling of the bulk solder ingots was experimentally were measured by K-
determined with thermocouples that recorded the temperature type thermocouples.
of the solder and the aluminum cooling block during After 5 min at 250 °C
solidification (see [9] for details). For all alloys an the ceramic was
undercooling of approx. 7 K (±4 K) was determined. This Figure 6: CAD drawing of the removed and cooled
value for undercooling is relatively small compared with punching tool down naturally by
measured values for small solder joints in [4, 10]. different thermal
masses and cooling methods (Fig. 9b). The cooling profiles
The influence of cooling rate on dendritic growth can be
with rates from 0.14 K/s to 10 K/s (mean value between
explained by temperature differences between the outer
240 °C and 140 °C) are shown in Fig. 7. A comparison of the
regions with better cooling and the centre area. The
different ball sizes is shown in Fig. 8.
temperature gradient increases with faster cooling and causes
the more directed growth. Table 1: Size of punched preforms and final ball diameters
An alternative experiment was carried out in order to PREFORMS SOLDER JOINTS
understand the mechanisms of dendritic growth. diameter height preforms volume diameter
For this experiment a solder ingot was solidified “bottom [µm] [µm] per joint [m³] [µm]
up” by different heating zones along the length of the test 2500 140 1 6,9E-10 1100
tube (see [9] for details). This way a temperature gradient was 700 140 2 1,1E-10 590
generated inside a large solder ingot. The results shown in 300 140 1 9,9E-12 270
Fig. 5 indicate a dendritic growth with the moving direction 100 140 1 1,1E-12 130
of the solidification front as it was expected [11]. The formed
dendrites reached lengths up to 10 mm. 250
melting point 217°C
200
temperature [°C]

150

100

50 -0.14 K/s
-1.1 K/s
-10.9 K/s
0
0 300 600 900 1200 1500 1800
time [s]
Figure 5: Influence of a generated temperature gradient inside Figure 7: Cooling profiles with mean gradients calculated
a solder sample on the dentritic growth of β-Sn in between 240 °C and 140 °C
SnAg3.0Cu0.5
The test matrix consisted of four alloys combined with
Experiments on small solder spheres three cooling rates.
Micro solder spheres were manufactured from raw solder. For each
Solder bars of the four investigated alloys (SnAg3.5 by JL combination four
Goslar, SnAg3.0Cu0.5 by Alpha Metals, SnAg3.8Cu0.7 by different ball sizes
Stannol and SnAg2.7Cu0.4Ni0.05 by JL Goslar) were rolled were prepared (see
to a foil with a thickness of 140 µm. Afterwards preforms Tab. 1). For each
with different diameter were punched out with the tool shown ball size six samples
in Fig. 6. The diameter of the preforms and the size of the were made and
final solder spheres are shown in Tab. 1. The samples were analysed (total
Figure 8: Comparison of
soldered without interface in order to prevent side effects and number of samples
investigated ball sizes
changes in composition. 288).

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Figure 9: Experimental procedure for reproducible cooling rates between 0.14 K/s and 10.9 K/s
Cross sections were prepared using SiC abrasive paper for the nucleation of the intermetallic and the nucleation of β-Sn
grinding. Polishing steps were done using diamond particles becomes longer. Therefore the intermetallic has more time to
of 3 µm and 1 µm and a colloidal silica suspension for final grow and becomes larger at slower cooling rates.
preparation. The microstructure was analysed by polarised
light microscopy and differential interference contrast (DIC)
in order to get information on grain orientation and phase
distribution.
In general, three types of microstructure can be found in
the investigated solder balls: large primary solidified
intermetallics (see Fig. 10), areas of dendritic growth with
major grain orientations (see Fig. 11) and areas of small,
randomly orientated grains with small precipitations (Fig. 11).
The areas with small grains differ from the eutectic solidified
regions found in the bulk SnAg3.8Cu0.7 solder (Fig. 3b). The
regions found in bulk specimen show no small, randomly
orientated grains. The coarse, dendritic areas are represented
by a major grain orientation, which indicates the growth
direction. It could be concluded, that such a region represents
a single grain, but it has to be considered, that small angle tilts
of grains cannot be analysed by the contrast of polarised light.
It has to be taken into account that balls, which were
solidified under similar conditions appeared to be completely Figure 10: Primary intermetallic formed in SnAg3.0Cu0.5
different (Fig. 14). Sometimes those balls seem to solidify solder ball (Ø 1100 µm) cooled with 0.14 K/s
with coarse, dendric areas and sometimes with small,
randomly, orientated grains. It is also possible that a solder The influence of cooling rate on the dendritic growth of
bump consists of both types of grain structures. β-Sn is somewhat ambiguous. There are different growth
directions found in a single ball (Fig. 11) and the cross section
Influence of cooling rate provides only the information of a single plane. This causes a
Fig. 10 shows the formation of a primary solidified Ag3Sn large variation of different shapes. However, no significant
intermetallic in the SnAg3.0Cu0.5 solder. However, the tendency of the dendritic growth has been observed by
formation of an intermetallic of that size compared to the changing the cooling rate. The eutectic regions between the
solder volume has not been investigated in the bulk specimen dendrites show also no effect by changing the cooling rate.
of the same solder alloy. The change in cooling rate showed These effects do not correspond with the conclusions made
that the growth of large, primary solidified intermetallics can for bulk solder ingots.
be minimized by faster cooling. All investigated alloys The influence of cooling rate on grain orientation is
showed no large intermetallics at the highest cooling rate of shown in Fig. 14. The influence of cooling rate on grain
10.9 K/s, what agrees with the results presented in [10, 12]. orientation seems to decrease with smaller solder volume.
The nucleation of Ag3Sn seems to need less undercooling Only the largest ball size shows small effect on cooling rate.
than β-Sn. By decreasing the cooling rate, the time between

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In these balls the appearance of regions with small, randomly
orientated grains is more frequent if cooling becomes faster.
These results indicate that the influence of cooling rate in
small solder bumps is different compared with the effects
found in bulk specimen. Apart from the effect on the growth
of large primary intermetallics, it can be concluded that the
influence of cooling rate becomes less important with
decreasing solder volume. This might be caused by a change
in the solidification conditions, which are influenced by the
undercooling of the β-Sn phase.
different grain sizes is found in SnAg3.5, while in the
SnAg3.0Cu0.5 solder only large or small grains can be found.
Fig. 16 also indicates that the size of the smallest grains is
slightly larger for SnAg3.5.
The SnAg3.0Cu0.5 solder and the SnAg2.7Cu0.4Ni0.05
solder behave similar for small solder balls (Ø 270 µm and
Ø 130 µm). The difference is seen especially for large
SnAg2.7Cu0.4Ni0.05 solder balls (Ø 590 µm and

Figure 11: Polarised light image showing the grain

orientation of a SnAg3.0Cu0.5 solder ball (Ø 1100 µm)
cooled with 1.1 K/s. Large areas with major grain orientations
mark dendritic growth. The centre region consist of small,
randomly orientated grains.
Influence of solder volume Figure 12: Volume effect on grain distribution and grain size
In general, there are two effects observed that indicate a of SnAg3.0Cu0.5 solder balls cooled with 1.1K/s
finer microstructure with decreasing solder volume.
The first effect is shown in Fig. 12 and Fig. 14. With
decreasing solder volume the appearance of small, randomly
orientated grains becomes more frequent. Large solder balls
mainly consist of coarse, dendritic regions with large grains.
In these balls only a few regions with small grains can be
found. The opposite effect can be observed in a small solder
volume. These balls mainly consist of small grains with
nearly no coarse, dendritic areas.
The second effect of solder volume on microstructure is
shown in Fig. 13. The size of the β-Sn dendrites increases
with smaller solder volume. In the smallest sample (Fig. 13d)
no dendritic structures can be found. This ball mainly consists
of small intermetallics surrounded by the Sn matrix.
Influence of solder composition
Fig. 15 shows how the general grain structure is
influenced by solder composition and ball size. Small changes
in alloy composition have strong effects on the grain
orientation and size.
The SnAg3.5 solder looks different compared with the Cu
containing solders (Fig. 15-16). The grain size in the SnAg3.5 Figure 13: Scaling effect on dendritic growth in
solder varies more continuously from small to large SnAg3.0Cu0.5 solder balls of different sizes
(Fig. 16a), while in the SnAg3.0Cu0.5 solder this change is
much more abrupt (Fig. 16b). That means a large variety of
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Figure 14: Effect of cooling rate and solder volume on the grain distribution and orientation of SnAg3.0Cu0.5 solder spheres
with different size

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Figure 15: Influence of solder composition on grain distribution and orientation of SnAgCu+ solder spheres cooled with 1.1 K/s

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Figure 16: Comparison of the grain structure of a) SnAg3.5
and b) SnAg3.0Cu0.5 solder balls (Ø 1100 µm) cooled with
1.1 K/s
Ø 1100 µm) that solidify with a coarser grain structure
compared to the SnAg3.0Cu0.5 solder spheres. This indicates
that the volume effect is suppressed.
The SnAg3.8Cu0.7 solder solidifies with the coarsest
microstructure of all investigated alloys. The balls shown in
Fig. 16 indicate that the volume effect is strongly suppressed.
Only a few of the smallest balls (Ø 130 µm) show areas with
small grains. The larger solder spheres solidify with large
grains in most of the cases. The grain orientations of these
grains do not show strong differences, what is indicated by
the poor contrast.
The grain structure of SnAg3.0Cu0.5 shows highly
symmetric orientated grains with large tilt angles, which are
represented by the strong contrast in Fig. 17.
The SnAg2.7Cu0.4Ni0.05 solder was the only alloy that
did not show large primary solidified intermetallics, even at
slow cooling rates. This is caused by the low Ag content in
the solder.
The compositional effect on the grain structure has been
investigated in [12]. This study points out that a small change
of the Cu content has strong influence on the size of grains.
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Figure 17: Appearance of regions with fine grain structure in
SnAg3.0Cu0.5 solder balls (Ø 1100µm) cooled with 10.9 K/s
a) multiple areas in one ball b) ring shaped area
An increase of the Cu content results in the formation of
larger grains. In [1] it is also mentioned that a higher Cu
content supports the dendritic growth.
Discussion
In Fig. 18, the microstructure of a SnAg3.0Cu0.5 ball
(Ø 1100 µm) cooled with 1.1 K/s is shown. Fig. 18 represents
different information of the same regions of the solder sphere:
The upper line (Fig. 18a-c) shows the grain orientation of the
ball. The lower line (Fig. 18d-f) shows the corresponding
microstructure.
The grain orientation of the ball (Fig. 18a) is divided into
two completely different areas. There is a fine structured
region with small randomly, orientated grains (Fig. 18b). This
region is surrounded by six large, coarse areas characterized
by three major grain orientations, which are represented by
the different greyscales (black, grey, white - Fig. 18a,
Fig. 18c). Theses major grain orientations also correspond
with those orientations found in the fine structured region
(Fig. 18b). Fig 18b and Fig 18e show details of the fine
structured area. It can be seen, that the microstructure
coarsens from inside out, i.e. the grain size and the size
Figure 18: Grain orientation (a, b, c: polarised light microscopy) and corresponding microstructure (d: bright field microscopy;
e, f: Differential Interference Contrast) of an as cast SnAg3.0Cu0.5 solder ball with Ø 1100µm, cooled with 1.1 K/s
of the intermetallics increase from the inside of this region to
the outside. At the edge of this area β-Sn dentrites can be
found and the fine microstructure suddenly turns into coarse
and conical growing areas with major grain orientations.
Fig. 18a also shows that those coarse areas expand with
increasing distance from the fine structured region. Fig. 18c
and Fig. 18f show details on the microstructure of the coarse
area. It consists of β-Sn dendrites with eutectic solidified
regions in between.
Furthermore, Fig. 18a shows that the grain orientation of
the coarse, dendritic areas is mirrored by the fine structured
region. That means that opposite dendrites have the same
grain orientation. This phenomenon is described as cyclic
twinning [14]. That means that the areas of different grain
orientations form twins.
Interpretations of the results, which are shown in Fig. 18,
allow a possible reproduction of the solidification process of
the solder ball. The fact that the coarse areas (Fig. 18a) grow
conical and expand with increasing distance from the fine
structured region allows the conclusion that solidification
starts with the fine structured areas. In [12] it is pointed out
that the nucleation for cyclic twinning starts at the vertex of
the twinning circle. This corresponds with the made
assumption. The subsequent dendritic growth depends on
conditions that have to be fulfilled for the surrounding melt.
These conditions for dendritic growth seem to be less often
reached in small solder volumina.
This fine structured region has not to be spherical or in the
centre of the ball. Other investigated SnAg3.0Cu0.5 solder
balls showed multiple, independent, fine structured regions
(Fig. 17a) or ring shaped areas (Fig. 17b). It is not clear where
in the sphere the initial nucleation of these regions starts,
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because it is reasonable to assume a turbulent flow inside the
ball.
A comparison between the microstructure of the large
solder ingots and the small solder balls reveals strong
differences even at similar cooling rates and solder
compositions.
These differences indicate a change in solidification
behaviour. The results of the experiments on bulk solder
ingots allow the assumption that large solder volumina
behave more similar to the phase diagram [13] than small
volumina. A possible explanation is the dependence of the
nucleation of β-Sn on undercooling. Undercooling becomes
larger with the decrease of solder volume [7]. This leads to
the conclusion that kinematical factors on the solidification
become more dominant in small solder balls than thermo-
dynamical factors. This might also be responsible for the
volume depending, scaling effect on the size of β-Sn
dendrites in the solder spheres.
Conclusions
Solidification experiments with different cooling rates
have been carried out on SnAgCu based specimens with
different volume: bulk solder ingots (V≈1E-06 m³) and solder
spheres with different sizes (Ø 1100 µm - V≈1E-09 m³;
Ø 590 µm - V≈1E-10 m³, Ø 270 µm - V≈1E-11 m³ and
Ø 130 µm - V≈1E-12 m³).
The solidification of the microstructure of SnAgCu
solders in dependence of the parameters cooling rate, solder
volume and solder composition is very complex. These
parameters are not independent from each other. The results
of the experiments show that the microstructure becomes finer
with smaller solder volume.
 The experiments on bulk solder ingots show strong
changes in microstructure at faster cooling. An increase of
cooling rate minimizes the size of intermetallics, decreases the
spacing of β-Sn dendrites and enlarges the areas of small
precipitations. Changes in solder composition cause the
primary solidification of different phases. An Ag content
above 3.5 wt.% causes the formation of large primary Ag3Sn
intermetallics. SnAgCu solders with more than 1 wt.% Cu
solidify with large primary Cu6Sn5 intermetallics in the
microstructure. Experiments on directional solidification have
been carried out in order to investigate the growth of β-Sn
dendrites. The formation of this phase can be directed by
temperature gradients inside the solder.
Experiments on small solder balls have been carried out at
different cooling rates (0.14 K/s, 1.1 K/s and 10.9K/s). Faster
cooling minimizes the size of primary solidified
intermetallics. There are no indications that cooling rate has
influence on the dendritic growth or on the size of areas with
small intermetallic precipitations. The influence of cooling
rate on grain structure becomes less important with decreasing
solder volume. Solder composition has influence on the
growth of primary intermetallics. Solder balls with a Ag
content below 3 wt.% solidified without primary Ag3Sn
plates, independent from cooling rate. Solder composition
also causes changes in the grain structure. Small changes in
solder composition determine whether a solder ball solidifies
with only a few, large grains or with a large number of small
grains. By decreasing the solder volume the formation of
small, randomly orientated grains becomes more frequent.
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