1241

Effects of Reflow on Wettability, Microstructure

and Mechanical Properties in Lead-Free Solders Journal of ELECTRONIC MATERIALS, Vol. 29, No. 10, 2000
(Received March 14, 2000; accepted June 6, 2000)
Special Issue Paper
1241
INTRODUCTION
In electronics technology, the basic functions of
solders have changed in recent years. Not only must
solders function in their traditional role as reliable
electrical interconnects; solder materials must also
have structural integrity, particularly, in surface
mount technology applications. Solders must also
perform in more robust environments consisting of
higher temperature and more severe mechanical load-
ings. To meet the ever-demanding challenges, lead-
free solders such as tin-silver solder alloys have re-
ceived considerable attention. Lead-free solders lack
the toxicity problems associated with leaded solders.
However, unlike leaded solders, the recently em-
ployed lead-free solders do not have a long history and
well-established manufacturing and engineering da-
tabase. Consequently, the inertia for acceptance of
lead-free solders by design engineers and manufac-
turers will remain pending a thorough examination of
these materials. However, research studies in recent
years
1
characterizing various properties and perfor-
mance of lead-free solders have alleviated some of the
reluctance for acceptance.
Typically, the electronics industry involves mul-
tiple-pass solder operations in which the solder is
reflowed. In such operations, wettability of the solder
materials is of extreme importance. Investigations
Effects of Reflow on Wettability, Microstructure
and Mechanical Properties in Lead-Free Solders
F. GUO, S. CHOI, J.P. LUCAS, and K.N. SUBRAMANIAN
Michigan State University, Department of Materials Science and Mechanics,
East Lansing, MI 48824-1226
Solder joints used in electronic applications undergo reflow operations. Such
operations can affect the solderability, interface intermetallic layer formation
and the resultant solder joint microstructure. These in turn can affect the overall
mechanical behavior of such joints. In this study the effects of reflow on
solderability and mechanical properties were studied. Nanoindentation testing
(NIT) was used to obtain mechanical properties from the non-reflow (as-melted)
and multiple reflowed solder materials. These studies were carried out with
eutectic Sn-3.5Ag solders, with or without mechanically added Cu or Ag rein-
forcements, using Cu substrates. Microstructural analysis was carried out on
solder joints made with the same solders using copper substrate.
Key words: Sn-3.5Ag solders, Cu substrates, microstructure, lead-free solder
dealing with wettability issues of Pb-free solders have
been conducted
28
and ongoing research is moving at
a rapid pace. Vianco and others
2,3
have found the
wetting characteristics of Sn-Ag based lead-free sol-
der to be comparable to leaded solder on copper
substrate. The wettabilty of gold substrate with eu-
tectic Sn-Ag solder has been shown to be commensu-
rate to that of Pb-Sn solder alloys.
4
The wetting
characteristics of any particular solder alloy are
strongly influenced by the flux used.
5,8
In particular,
the wetting parameters, such as interfacial tension
and wetting rate, of eutectic Sn-Ag solder can be
highly variable depending on the choice of flux.
5
In this study, the effects of solder reflow on wettabilty
characteristics, microstructure, and mechanical prop-
erties were investigated. Multiple-reflow experiments
were conducted using eutectic Sn-3.5Ag non-compos-
ite and eutectic Sn-3.5Ag based composites with me-
chanically-added, fine Cu and Ag particles on a copper
substrate. The motivation to conduct this investiga-
tion on reflow characteristics of composite solders
was due to limited published literature. It is also
believed that the composite approach to engineered
solder properties should be advanced.
9
EXPERIMENTAL PROCEDURES
Preparation of Testing Materials
The composite solders were prepared by mechani-
cally adding ~6 m size Cu or ~4 m size Ag particles
1242 Guo, Choi, Lucas, and Subramanian
to the Sn-3.5Ag eutectic solder paste. The reinforcing
particles were blended with self-fluxed Sn-3.5Ag eu-
tectic solder paste in a ceramic crucible. To achieve a
uniform distribution of the reinforcing phase in the
eutectic solder matrix, a mixing time of at least 15 min
was used.
Copper and silver powders used as the reinforce-
ments were obtained from Atlantic Equipment Engi-
neers, Inc., Bergenfield, New Jersey. The purity of
both materials was 99.9%. The morphology and size of
as-received Cu and Ag particles were previously stud-
ied with the scanning electron microscope (SEM), and
have already been reported.
10
In order to study the effects of volume fraction of the
reinforcing phase and to evaluate the role of different
reinforcements, composite solders with 6, 12, and
17.5 volume percent Cu particles and 17.5 volume
percent Ag particles were prepared.
Wetting Experiments
The copper substrates with these dimensions, 2 cm
2 cm 1.5 cm, were chemically cleaned with a solution
of 50% nitric acid and 50% H
2
O before each experi-
ment. Reflow specimens were made first by preparing
disc-shaped solder paste preform. This was accom-
plished by flowing the solder paste through an orifice
of 5 mm in diameter and then cut to size using a razor
blade. With this method, consistent size discs weight-
ing approximately 0.3 grams were achieved for the
subsequent melting and reflow process.
All the disc-shaped solder preforms were placed on
copper substrates for melting on a hot plate. Reflow
experiments were carried out by remelting solder
materials on the same copper substrate for at least 3
times without refluxing to better mimic industrial
practice. The thermal history profile for initial melt-
ing and subsequent reflow experiments is shown in
Fig. 1. Specimens were heated to a maximum tem-
perature of 280C and then placed on a chill alumi-
num block to cool to room temperature. Upon solidifi-
cation, all specimens exhibited a spherical-cap shape.
Non-reflow (as-melted) and reflowed samples were
cleaned, sectioned, polished and examined using op-
tical and scanning electron microscopy to determine
the wetting angles. Image processing software was
used to measure the wetting angles from the SEM
micrographs. This technique for determining contact
angles provided consistent results similar to those
previously published.
9
Reflow Experiments on Solder Joints
The effect of reflow on the microstructure of solder
joints was also investigated. Single shear lap joint
specimens were made by soldering two dog-bone
shaped copper strips with eutectic Sn-3.5Ag solder
paste as well as composite solder paste containing
17.5 vol.% Cu or Ag reinforcements. Details about the
dimensions and fabricating methods of the solder
joint can be found elsewhere.
11
The nominal soldered
area dimensions were 1 mm 1 mm. The final solder
joint for reflow analysis had a nominal thickness of
about 80~100 microns.
Reflow analysis was carried out by remelting the
solder joints in aluminum fixture on a hot plate for at
least 3 reflows at 280C. The thermal history profile
for the reflow experiment on the solder joints is shown
in Fig. 2. In the SEM analysis of all solder joint
samples, particular interest was focused on the for-
mation and growth of intermetallic layers around Cu
and Ag particle reinforcements in the composite sol-
der and at the copper substrate-solder interface.
RESULTS AND DISCUSSION
Effect of Reflow on the Wettability
of Non-Composite and Composite Solders
Results of wetting angles measured as a function of
reflow conditions are shown in Table I. Results in
Table I indicate that eutectic Sn-3.5Ag solder paste
has the best wettability of all non-reflow solders with
an average contact angle of about 10.5. The wetting
angle determined in this study using solder paste
preforms was compared to that determined using
solid solder preforms of a previous study.
9
The results
of this study indicate that the wetting angle of eutec-
Fig. 1. Temperature profile of solder/copper wettability experiment.
Fig. 2. Temperature profile of reflow experiment on solder joints.
1243
Effects of Reflow on Wettability, Microstructure
and Mechanical Properties in Lead-Free Solders
tic Sn-3.5Ag solder paste is about 8 smaller than the
eutectic Sn-3.5Ag solid solder preform, where the
nominal wetting angle was typically around 18. The
wetting angle for non-reflow composite solder with
17.5 vol.% Cu particle was significantly higher, ap-
proximately 47. However, composite solder with com-
parable volume fraction of Ag reinforcement exhib-
ited a wetting angle of about 21.
As indicated in Table I, there is no statistically
meaningful difference in the wetting angles between
non-reflow and multiple-reflowed solder materials.
The wettability ranking of these materials is shown in
the last column of Table I and schematically illus-
trated in Fig. 3. The non-reflow and reflowed solder
produced spherical caps of the solder on the substrate.
It is contended that the eutectic Sn-3.5Ag solder
paste has the best wettability due in part to the way
in which the solder paste is manufactured. The self-
fluxed paste would tend to prevent formation of oxide
that can be detrimental to wettability. A rough esti-
mation of the amount of flux that encompasses the
particles of the solder paste was approximately
12 wt.%. Apparently, fluidity is therefore enhanced
giving a significantly lower contact angle.
As noted previously, the Cu composite solder showed
the highest contact angle and hence the least wet-
table. To ascertain the variation in contact angle with
reinforcement content, we conducted a collateral ex-
periment where the volume fraction of mechanically
added Cu particle reinforcements ranged from 6 to
17.5 vol.%. For non-reflow Cu composite solders, Fig.
4, the wetting angle increased with the increase of the
volume fraction of Cu reinforcements. At the lowest
volume fraction of 6 vol.%, the wetting angle was 18
whereas at 17.5 vol.% the wetting angle increased to
47. The propensity for the Cu reinforcement to form
Cu
6
Sn
5
intermetallics apparently affects the flow prop-
erties of this composite solder. Similar to our previous
studies,
10
we find that ~6 micron size Cu particle
reinforcements will be converted to Cu
6
Sn
5
interme-
tallics after 34 reflows. Due to the prolific growth of
the Cu-Sn intermetallic layer around the Cu rein-
forcements, the effective volume fraction is enhanced,
even for the as-melted composite solder. For example,
after three reflows, the effective volume fraction be-
comes approximately twice that of the as-mixed rein-
forcement volume fraction of the solder paste. One
might envisage that the Cu reinforcements could act
to increase the interfacial surface tension with the
molten solder (chemically constrained) thus reducing
Table I. Wetting Angles as a Function of Reflow Conditions (Angles Measured in Degrees)
Materials Conditions Angle 1 Angle 2 Angle 3 Angle 4 Average 1* Average 2**
Eutectic- as-melted 13.6 8.1 9.5 10.6 10.45 10.5 2
Sn-3.5Ag reflow 1 11.4 7.9 6.1 10.9 9.08 12.1 3.9
(paste) reflow 2 21.3 9.9 15 15.40
reflow 3 14.4 8.6 14.7 9.8 11.88
Cu composite as-melted 43.3 51.1 52.6 42.2 47.30 47.3 5.3
solder reflow 1 57.1 48.7 55.8 28.1 47.43 44.1 10
reflow 2 38.2 37.9 37 44.6 39.43
reflow 3 33.4 49.1 65 34.8 45.58
Ag composite as-melted 25.7 17.3 22.3 19.2 21.13 21.1 3.2
solder reflow 1 19.4 22.6 12.1 11.4 16.38 18.5 4.6
reflow 2 23.5 21 19.3 9.7 18.38
reflow 3 21.4 23.1 14.7 23.9 20.78
Eutectic- as-melted 18.2 17.8 19.2 16.8 18.00 18.0 0.9
Sn-3.5Ag reflow 1 22.5 18.9 20.7 20.7 20.70 9.6 3.4
(preform) reflow 2 25.3 23.7 19.7 21.3 22.50
reflow 3 16.4 15.7 15.3 14.6 15.50
*Average 1 is the average of all the angle measurements under each different condition.
**Average 2 basically averages the angles in the multiple-reflow experiment to compare with the non-reflow conditions.
Fig. 3. Schematic drawing of wetting properties of different solder
materials observed in the reflow experiment.
1244 Guo, Choi, Lucas, and Subramanian
flow on the substrate. Also, there can be a geometric
effect where the Cu particles prevent contact of the
molten solder with the Cu substrate and/or inhibit
flow of the leading edge of the spreading spherical cap
which can lead to decrease in wettability. Also, Cu
particles modified by the growth of Cu-Sn intermetal-
lic layer will tend to constrain the advancing edge of
the molten solder cap.
It is also significant that Ag particle reinforced
composite solder at 17.5 vol.% did not show a high
wetting angle as observed in Cu particle reinforced
composite solder. In contrast to Cu reinforcements
that form a thick Cu-Sn intermetallic layer, Ag rein-
forcements form only a thin, Ag
3
Sn intermetallic
boundary layer. Moreover, there is no significant
increase in the effective volume fraction due to the
reflow process. Apparently, wettability of composite
solder is not significantly affected when the effective
Fig. 4. Changes of wetting angles with the volume fraction of the
copper particles in the Cu particle reinforced composite solders (non-
reflow).
a b
c d
Fig. 5. Effect of reflow on the growth of Cu-Sn intermetallics around Cu
particle reinforcements: (a) non-reflow, (b) first reflow, (c) second
reflow, and (d) third reflow.
Fig. 6. Effect of reflow on the growth of Ag
3
Sn intermetallics around Ag
particle reinforcements: (a) non-reflow, (b) first reflow, (c) second
reflow, and (d) third reflow.
a b
c d
Fig. 7. The growth of intermetallic layer around Cu and Ag reinforce-
ment particles due to reflow. There is virtually no growth of Ag-Sn
intermetallic layer around the Ag reinforcement.
1245
Effects of Reflow on Wettability, Microstructure
and Mechanical Properties in Lead-Free Solders
reinforcement volume fraction is approximately
20 vol.% or less. Similar wetting angles of around
1820 were observed in a composite solder contain-
ing 20 vol.% non-coarsening in situ Cu
6
Sn
5
reinforce-
ments fabricated in our laboratory.
9
Also, it was found that reflow had no noticeable
influence on contact angle of the solder materials inves-
tigated. However, it is worth noting that upon reflow
the substrate being rewetted is the Cu
6
Sn
5
interme-
tallic layer rather than the actual Cu substrate.
Effects of Reflow on Microstructure of
Composite and Non-Composite Solder Joints
Intermetallic Layer Around
the Particulate Reinforcements
The microstructure representative of Cu particle
reinforced composite solder joints is shown in Fig. 5.
The intermetallic layer (light contrast) circumscribes
the core region (dark-contrast) representing the un-
converted Cu particles. This intermetallic formed
around the Cu reinforcements consists of a bi-layer
structure of Cu
3
Sn (-phase) and Cu
6
Sn
5
(-phase).
Typical microstructures of Ag particle reinforced com-
posite solders are shown in Fig. 6. Unlike Cu compos-
ite solders joint, an extremely thin intermetallic layer
of Ag
3
Sn forms around the Ag particle reinforcements.
The extent of intermetallic layer growth with reflow
is depicted in Fig. 5ad. Upon reflow, the intermetal-
lic layer around the Cu particles grew dramatically
while the Cu particle was being converted to more Cu-
Sn intermetallics. Complete conversion of the copper
reinforcement was observed usually after about three
reflows. The effect of reflow on the growth of Ag
3
Sn
intermetallics around Ag particle reinforcements is
shown in Fig. 6. Very little coarsening of the Ag
particles was observed due to the slow growth of the
Ag
3
Sn intermetallic. The extent of growth of the
intermetallic layer around the reinforcements due to
reflow is demonstrated in Fig. 7. The vast difference
in the intermetallic layer growth around Ag and Cu
particle reinforcements is related to the difference in
diffusivities of elemental Cu and Ag in Sn. In the solid
state, Cu diffuses nearly 1000 times faster in body
centered tetragonal (BCT) Sn (perpendicular to its c-
axis) axis than does Ag,
12
thus promoting enhanced
intermetallic layer growth. The rate is expected to be
even faster in molten materials.
Interfacial Intermetallic Layer
in Composite Solder Joints
The effect of reflow on the formation and growth of
Cu-Sn intermetallic layer at the solder/copper sub-
strate interface in the Cu reinforced composite solder
joint is shown in Fig. 8. Significant interfacial layer
growth was observed. For non-reflow solder joints,
the initial solder/copper substrate interfacial layer
thickness was 1.9 m, while the layer thickness in-
a b
c d
Fig. 8. Effect of reflow on the growth of Cu-Sn intermetallic layer at Cu
substrate-solder interface in Cu reinforced composite solder joint:
(a) non-reflow, layer thickness = 1.89 m, (b) first reflow, (c) second
reflow, and (d) third reflow, layer thickness = 4.43 m.
a b
Fig. 9. Effect of reflow on the growth of Cu-Sn intermetallic layer at Cu
substrate-solder interface in Ag reinforced composite solder joint:
(a) non-reflow, layer thickness 1.26 m, (b) first reflow, (c) second
reflow, and (d) third reflow, layer thickness = 2.53 m.
c d
1246 Guo, Choi, Lucas, and Subramanian
creased to 4.4 m after only three reflows. The layer
thickness increased 2.4 times after three reflows. The
influence of reflow on the interfacial intermetallic
layer at the solder/copper substrate interface in the
Ag particle reinforced composite solder joint is pre-
sented in Fig. 9. The initial layer thickness was 1.3 m.
Subsequent to three reflows, the layer thickness in-
creased by a factor of 2. In general, the overall thick-
ness of the interfacial layer in the Ag composite solder
joint was ~1/2 of that in the Cu composite solder joint
after multiple reflows. That the overall interfacial
layer thickness of the Ag reinforced composite is
about half that of Cu reinforced composites has impli-
cations regarding the reliability of solder joints. For-
mation and growth of the brittle interfacial Cu-Sn
intermetallic layer in solder joints has been linked to
joint failure.
13
Effects of Reflow on the Microstructure
of Eutectic Sn-3.5Ag Solder Joints
The microstructure of eutectic Sn-3.5Ag solder joints
as a function of reflow is shown in Fig. 10. The
microstructure in Fig. 10a for non-reflow solder is
characterized by Sn cells separated by wide bands of
eutectic Ag
3
Sn. With multiple reflows, the Ag
3
Sn
bands separating the Sn cells became narrower and
simultaneously the size of the Sn cells increased as
exhibited in Fig. 10bd.
The effect of reflow on the interfacial intermetallic
layer in the eutectic Sn-3.5Ag solder joint is illus-
trated in Fig. 11. The interfacial layer grew with
reflow from the initial layer thickness of 1.7 m to a
final layer thickness of 4.3 m. The interfacial layer
grew by a factor of 2.5 after reflow. This is very similar
to the interfacial intermetallic layer growth behavior
that occurred during reflow in the Cu particle rein-
forced composite solder joints as shown in Fig. 12.
Figure 12 compares the growth of interfacial layers
at the copper substrate in all the solder joint materi-
als studied.
Effect of Reflow on Mechanical
Behavior of Solder
Reflowing of the solder materials, particularly sol-
der joints on circuit boards, is required in manufac-
turing processes. Two or three reflows are considered
normal for a typical wave soldering process. To assess
whether multiple-reflow of solder materials will af-
fect the resultant mechanical properties, nanoinden-
tation testing (NIT) was performed on eutectic Sn-
3.5Ag solder. NIT was conducted on eutectic solders
reflowed up to 3 times using the Nano Indenter

XP
mechanical properties microprobe (MPM) from MTS
Corporation. With the MPM, simultaneous measure-
ment of indenter penetration depth and load makes it
possible to determine certain mechanical properties.
Mechanical properties assessed were hardness, modu-
lus and creep properties. The most significant finding
with regards to mechanical properties change turned
out to be the decrease in hardness as a function of
Fig. 10. Effect of reflow on the microstructure of eutectic Sn-3.5Ag non-
composite solder joint: (a) non-reflow, (b) first reflow, (c) second
reflow, and (d) third reflow.
a b
c d
a b
c d
Fig. 11. Effect of reflow on the growth of Cu-Sn intermetallic layer at Cu
substrate-solder interface in eutectic Sn-3.5Ag non-composite solder
joint: (a) non-reflow, layer thickness = 1.74 m, (b) first reflow, (c) second
reflow, (d) third reflow, layer thickness = 4.27 m.
1247
Effects of Reflow on Wettability, Microstructure
and Mechanical Properties in Lead-Free Solders
reflow as shown in Fig. 13. Also, the yield strength can
be estimated according to Tabor
14
from hardness
data. In Fig. 14, the relative change in yield strength
is shown as a function of reflow. On average, the yield
strength of eutectic Sn-3.5Ag solder is reduced by
~30%. The reduction in hardness/yield strength is
motivated by the change in solder chemistry and
microstructure due to the reflow process. It is sug-
gested that the composition of the solder changes
from the eutectic composition (96.5 Sn-3.5 Ag) to an
off-eutectic composition containing less Sn due to
reflow. The reduction in the amount of Sn is due to its
consumption in the formation of the intermetallic
layer consisting of Cu
6
Sn
5
and Cu
3
Sn compounds.
15
Change in solder microstructure is expected for off-
eutectic stoichiometry. Proeutectic Ag
3
Sn will pre-
cipitate out of the liquid first followed by solidification
at the eutectic composition with continued cooling. As
indicated in Fig. 10, the Sn cells became larger and
the necklace of eutectic Ag
3
Sn became narrower sub-
sequent to multiple reflows. The microstructure
Fig. 12. Comparison of interfacial intermetallic layer growth due to
reflow between Cu composite solder, Ag composite solder, and
eutectic Sn-3.5Ag non-composite solder joint.
Fig. 13. Change in hardness of eutectic Sn-3.5Ag solder as a function
of reflow.
Fig. 14. Change in yield strength of eutectic Sn-3.5Ag solder as a
function of reflow. yield strength decreases with multiple reflows.
Fig. 15. Microstructure of eutectic Sn-3.5Ag solder around indent:
(a) non-reflow solder, (b) three-reflow solder. The size of the Sn cells
is larger for reflowed materials. Correspondingly, the yield strength is
lower.
a b
Fig. 16. The effect of reflow on steady-state creep strain rate of eutectic
Sn-3.5Ag solder. The stress exponent is slightly higher for multiple
reflowed solder.
1248 Guo, Choi, Lucas, and Subramanian
around the indents of the non-reflow and 3 times-
reflowed solder is shown in Fig. 15. In Fig. 15a for non-
reflow solder, smaller Sn cells and wider Ag
3
Sn bands
were evident. Whereas, Fig. 15b showed larger Sn
cells and thinner Ag
3
Sn bands after three reflows.
The lower hardness and yield strength observed is
consistent with materials having a larger grain size.
Nanoindentation creep tests were conducted. As-
suming steady steady-state behavior, = A
n
, the
stress exponent for indentation creep was also deter-
mined for non-reflow and multiple-reflowed solder.
The stress exponent for eutectic Sn-3.5Ag solder ma-
terials after three reflows was n = 8, whereas the non-
reflow solder exhibited a value of n = 7.1. The stress
exponent data are shown in Fig. 16. The difference in
n-values suggests that creep deformation in the sol-
der is influenced by reflow history. From n values
obtained, the steady-state creep rate of reflowed sol-
der materials is higher due to reflow-induced micro-
structure and composition changes.
CONCLUSIONS
1. Eutectic Sn-3.5Ag solder showed the best
wettability of all the solder materials studied.
The wettability of 17.5 vol.% Ag-reinforced com-
posite solder was significantly better than 17.5
vol.% Cu-reinforced composite solder. Because of
profuse intermetallic layer growth around Cu
reinforcements, the effective volume fraction
doubled. Wettability can be improved, however,
by lowering the volume fraction of the reinforcing
phase, particularly Cu particles.
2. No significant changes in contact angles were ob-
served with multiple reflow of the solder materials.
3. The initial formation of Cu-Sn intermetallics
around the Cu reinforcements was considerable,
whereas the Ag
3
Sn intermetallic layer thickness
around the Ag reinforcements was minimal.
Growth of the intermetallic layer around the Cu
particle reinforcements was excessive leading to
total consumption of the Cu particles after 34
reflows. By comparison, no substantial conver-
sion of the Ag reinforcements into Ag
3
Sn interme-
tallics was evident after multiple reflows.
4. The microstructure of non-reflow eutectic Sn-
3.5Ag solder can generally be characterized by
small Sn cells surrounded by wide-banded eutec-
tic Ag
3
Sn phase. In comparison, the microstruc-
ture of multiple reflowed solder is characterized
by large Sn cells circumvented by a thin necklace
of eutectic Ag
3
Sn precipitates.
5. The hardness and yield strength of multiple
reflowed eutectic Sn-3.5Ag solder were reduced
by 30% after three reflows. This finding is com-
mensurate with the increasing size of Sn cells
produced by multiple reflow as a larger grain/cell
size that will exhibit a lower yield strength.
6. The stress exponent, n, determined using inden-
tation creep testing was about 7 for non-reflow
solders and about 8 for multiple reflowed solders.
From the stress exponents observed, the steady-
state creep rate for the multiple reflowed solder
will be higher compared to non-reflow solder.
ACKNOWLEDGEMENTS
The authors acknowledge the support of this work
from the State of Michigan Research Excellence Funds
administered through the Composite Materials and
Structures Center at Michigan State University. We
also thank Brandon Campbell for his assistance in
sample preparation and testing.
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