Journal of ELECTRONIC MATERIALS, Vol. 38, No.

1, 2009 Special Issue Paper

DOI: 10.1007/s11664-008-0554-9
Ó 2008 TMS

Effect of Cu Thickness on the Evolution of the Reaction

Products at the Sn-9wt.%Zn Solder/Cu Interface During
Reflow

CHIH-HAO CHEN,1 CHI-PU LIN,1 and CHIH-MING CHEN1,2

1.—Department of Chemical Engineering, National Chung-Hsing University, Taichung 402,

Taiwan, ROC. 2.—e-mail: chencm@nchu.edu.tw

Interfacial reactions between Sn-9wt.%Zn solder and Cu substrates at 230°C

were investigated. The substrate thickness was found to have noticeable
effects on the evolution of the reaction products formed at the solder/Cu
interface. The CuZn5 and Cu5Zn8 phases were formed at the early stage of
reflow, regardless of the Cu thickness, while, with increasing reflow time, the
two phases displayed different growth behaviors on the Cu substrates with
various thicknesses. For the thicker Cu substrates with a thickness of 6 lm,
10 lm, and 0.5 mm, CuZn5 disappeared but Cu5Zn8 kept on growing after a
longer reflow time. In contrast, for the thinner Cu substrates with a thickness
less than 3 lm, Cu5Zn8 shrank with increasing reflow time but CuZn5 grew
dominantly. A different evolution of the grain morphology of CuZn5 was also
observed between the thicker and thinner Cu substrates. When the reflow
time was increased, the CuZn5 grains retained a rounded shape on the thinner
Cu substrates; however, the grain structure became faceted on the thicker Cu
substrates.

Key words: Interfacial reaction, Sn-9wt.%Zn solder, Cu, substrate thickness

closer to that of the conventional Sn-37 wt.% Pb

INTRODUCTION
According to the Restriction of Hazardous
Substances in Electrical and Electronic Equipment
(RoHS) regulations, Pb has been banned from use in
electronic products since July 1, 2006.1 The major
impact is that the electronics industries have had to
find a replacement for the conventional Pb-con-
taining solders. Among many candidates, Pb-free
solders are recognized as the most appropriate
replacement, and their relevant properties have
been examined extensively. Various Pb-free solders
have been proposed, of which the Sn-9wt.%Zn
(denoted as Sn-9Zn hereafter) alloy attracts much
attention because of its lower cost, suitable mechan-
ical properties, and a melting point (198.5°C) that is
(Received February 19, 2008; accepted August 25, 2008;
published online October 8, 2008)
alloy (183°C).
Solders are generally used as joining materials to
connect components to the contact pads on printed
circuit boards. Because the contact pads are usually
made of metals, joints of solder/metal are formed
after soldering. To evaluate the joint reliability,
investigations of interfacial reactions between sol-
ders and metallic substrates are conducted.2–17
Cu is one of the most common contact pads in elec-
tronic products. Much effort has been devoted to the
investigation of the interfacial reactions between
Sn-9Zn solder and Cu substrates.10–17 Although Sn
and Zn can react with Cu to form Cu-Sn and Cu-Zn
intermetallic compounds, respectively, as suggested
in the binary phase diagrams,18,19 the primary
reaction products that have been reported in the
literature are Cu-Zn compounds.10–17 Three phases,
CuZn, Cu5Zn8, and CuZn5, may form at the inter-
face in the temperature range of soldering pro-
cesses, according to the binary Cu-Zn phase

61
62
diagram, but mostly only Cu5Zn8 can form.10–16
In previous reports,10–16 the Cu substrate was
usually in bulk form and, thus, the supply of Cu for
interfacial reactions was abundant. In our recent
work, it was found that CuZn5 becomes the domi-
nant reaction product when the Cu substrate is
converted to thin-film type with a thickness of only
4000 Å.17 Obviously, the Zn-rich CuZn5 phase
replaces the Cu5Zn8 phase when the supply of Cu is
limited. In other words, the thickness of the Cu
substrate should play an important role in the
Sn-9Zn/Cu interfacial reaction. To gain a detailed
understanding of the effect of Cu substrate thick-
ness on the Sn-9Zn/Cu interfacial reaction, we
investigated Cu substrates of various thickness in
the work now described. Since Cu substrates with a
thickness of 4000 Å and 0.5 mm were examined in
our previous work,17 to make a more detailed com-
parison, we have used part of those results in the
discussion here.
EXPERIMENTAL
Sn and Zn shot of 99.99% purity were used to
prepare the Sn-9Zn solder. Suitable amounts of Sn
and Zn shot were weighed according to the solder
composition and sealed in a vacuum quartz tube.
These shot were put into a furnace at 450°C for 72 h
to reach homogeneity. Then, the molten solder alloy
was quenched in ice water. A small piece of solder
(5 mg) was cut from the solidified ingot. The piece
was cleaned and placed on a flux-coated [rosin
mildly activated (RMA) flux] Cu substrate. Cu sub-
strates of five thicknesses were prepared: 4000 Å;
3 lm; 6 lm; 10 lm; and 0.5 mm. The 4000 Å Cu
substrate was prepared by sputtering a Cu thin film
of the desired thickness on an oxidized Si chip. To
improve adhesion of the Cu thin film with the oxi-
dized Si, a Ta thin film of 200 Å thickness was
sputtered prior to the Cu deposition. The Cu sub-
strates of thicknesses from 3 lm to 10 lm were
obtained by electroplating Cu onto an oxidized
Si chip after the above-mentioned Cu/Ta deposition.
A Cu plate 0.5 mm thick was purchased and then
cleaned, polished, and used directly.
To conduct the reflow reaction, we placed the Cu
substrate, with a solder piece on its surface, on a hot
plate at a constant temperature of 230°C. The
duration of reflow ranged from 1 min to 60 min.
After reaction, the sample was mounted in epoxy
resin and examined metallographically. The sample
was ground and polished to expose the cross-section
of the solder/Cu interface. Field-emission scanning
electron microscopy (FESEM) was used to observe
the microstructure of the solder/Cu interface. Field-
emission electron probe microanalysis (FEEPMA)
was used for the compositional analysis of the
reaction products formed at the solder/Cu interface.
The sample was also dipped into an etching solu-
tion, 93% CH3OH + 2% HNO3 + 5% HCl, to remove
the entire solder and expose the reaction products
C.-H. Chen, Lin, and C.-M. Chen
for top-view examinations. An image processing
system was used to measure the cross-sectional area
of the reaction products and the linear length of the
solder/Cu interface. We determined the average
thickness of the reaction products by dividing the
cross-sectional area by the linear length.
RESULTS
Figure 1 shows a series of scanning electron
micrographs of the solder/Cu interface after reflow
for 1–60 min.17 The thickness of the Cu substrate is
0.5 mm. Two compounds were formed at the inter-
face after reflow for 1 min, as shown in Fig. 1a.
According to the compositional analysis of FEE-
PMA, the compound adjoined to the solder was
identified as the CuZn5 phase and that adjacent to
the Cu substrate was Cu5Zn8. Upon increasing the
reflow time, the Cu5Zn8 phase grew at a much faster
rate than the CuZn5 phase, as seen in Fig. 1b and c.
This significant difference in the growth rates of the
two phases can also be seen in Fig. 2, which depicts
the relationship between the compound thickness
and the reflow time. Although the CuZn5 phase did
not display noticeable growth (compared with that
of the Cu5Zn8 phase), a remarkable change in its
grain structure is observed in Fig. 3a–c. The top-
view scanning electron micrograph in Fig. 3a
reveals that the grain size of the CuZn5 phase is
fairly uniform and the grain structure is rounded
after 1 min of reflow, while the grain size in Fig. 3c
becomes extremely non-uniform after 10 min of
reflow. Some grains grew as big as several
micrometers, while the rest remained smaller than
those shown in Fig. 3a. These bigger grains display
a faceted structure, which was different from the
initial rounded shape seen in Fig. 3a. After reflow
for 60 min, as seen in Fig. 1d, the CuZn5 phase
disappeared and only the Cu5Zn8 phase was found
at the interface. The top-view scanning electron
micrograph in Fig. 3d reveals that the Cu5Zn8
grains are fine and faceted.
Figure 4 comprises the scanning electron micro-
graphs of the solder/Cu interface after reflow, in
which the thickness of the Cu substrate is 10 lm.
After 10 min of reflow, as seen in Fig. 4a, two com-
pounds were formed at the interface. Electron probe
microanalysis (EPMA) indicated that the two com-
pounds were also CuZn5 and Cu5Zn8 phases. The
compound formation and grain structure are similar
to those in Fig. 1c for the Cu substrate of 0.5 mm
thickness. It can be seen that the Cu substrate was
not consumed completely. After reflow for 60 min,
only the Cu5Zn8 phase remained at the interface,
and the Cu substrate had been completely con-
sumed, as seen in Fig. 4b. The results from the Cu
substrate of 6 lm thickness are similar to those
from 10 lm thickness and, thus, are not shown
here.
When the thickness of the Cu substrate was
reduced to 3 lm, both the CuZn5 and Cu5Zn8 phases
Effect of Cu Thickness on the Evolution of the Reaction Products at the Sn-9wt.%Zn Solder/Cu
Interface During Reflow
Fig. 1. Scanning electron micrographs of the solder/Cu interface
after reflow at 230°C for (a) 1 min, (b) 5 min, (c) 10 min,17 and
(d) 60 min,17 in which the thickness of the Cu substrate is 0.5 mm.
were also formed at the solder/Cu interface after
reflow for 5 min, as seen in Fig. 5a. Meanwhile, the
Cu substrate had been completely consumed. After
reflow for 60 min, the two compounds still existed at
63
the interface, as seen in Fig. 5b, but the compoundsÕ
thickness and phase structure differed from those in
Fig. 5a. The Cu5Zn8 phase had shrunk, while the
CuZn5 phase had grown thicker and displayed a
scallop-type structure. Figure 6 shows the scanning
electron micrographs of the solder/Cu interface for
the Cu substrate of 4000 Å thickness, which had
been reported in our previous work.17 It was seen
that the Cu thin film had been completely consumed
after reflow for only 1 min, and a compound layer
had been formed at the interface. Based on careful
scanning electron microscopy (SEM) observation,
this compound layer was actually composed of two
different phases. The upper phase (adjacent to the
solder) was thicker and was identified as the CuZn5
phase. Another phase adjacent to the Si chip was too
thin to be observable under the SEM magnification
as shown in Fig. 6a. Such thinness made the com-
position of this phase difficult to be determined,
while we had determined that this thin phase was
Cu5Zn8 using x-ray diffraction (XRD) in our previ-
ous work.17 After reflow for 10 min, the Cu5Zn8
phase disappeared and only the CuZn5 phase
existed at the interface, as seen in Fig. 6b. The
disappearance of the Cu5Zn8 phase was also con-
firmed by the XRD results.17 Similar to Fig. 5b, the
CuZn5 phase presented a scallop-like structure.
Top-view examination in Fig. 7 reveals that the
CuZn5 grains are rounded.
DISCUSSION
Morphological Evolution of the CuZn5 Grain
As seen in Fig. 3, the CuZn5 grain size is uniform
for a shorter reflow time but gradually becomes non-
uniform with increasing reflow time. The bigger
grains in Fig. 3c are likely to have preferential
growth orientations, since they exhibit a faceted
structure and grow at a much faster rate than the
rest of the smaller grains. The presence of a faceted
grain structure and preferential growth orienta-
tions suggests that the interfacial energy between
the CuZn5 phase and the molten solder is likely to
be anisotropic. For a shorter reflow time, as seen in
Fig. 3a, however, the CuZn5 grains exhibit a roun-
ded shape, suggesting that the interfacial energy at
the early stage of reflow is likely to be isotropic. The
above comparison implies that the type of interfa-
cial energy of the solder/CuZn5 interface has a
strong dependence on the length of reflow time.
During the solder/Cu interfacial reaction, Cu-Zn
compounds are formed at the interface and simul-
taneously consume Zn in the solder. At the early
stage of reflow, Zn consumption is insignificant,
because the Cu-Zn compounds are thin. Hence, the
solder composition near the interface could be very
close to the initial Sn-9Zn composition. When the
reflow time is increased, more Zn atoms are con-
sumed with the growth of the Cu-Zn compounds,
and the solder composition will change accordingly.
To understand the change of the solder composition,
64
Fig. 2. Relationships between the compoundsÕ thicknesses and the reflow time.
we produced scanning electron micrographs of lower
magnification, as seen in Fig. 8, to display the
interior microstructure of the solder. Obviously, the
microstructure is significantly changed with
increasing reflow time, indicating that the solder
composition indeed changes. Shown in Fig. 9 is the
Sn-rich region of the Sn-Zn binary phase diagram.19
The eutectic SnZn alloy contains 91.2 wt.% Sn and
8.8 wt.% Zn, so the initial composition of the solder
is in the hypo-eutectic region. As the solder is cooled
after reflow, the solidification path will follow the
line (A), so the primary Zn phase would precipitate
out first. From the microstructure observation of
Fig. 8a, it can be seen that, before 5 min of reflow,
primary Zn precipitates (black spots) exist in the
solder, suggesting that this solder composition is
located in the hypo-eutectic region. When the reflow
time is increased, more Zn atoms are consumed with
the growth of the Cu-Zn compounds. The solder
composition would change and might shift to the
hyper-eutectic region, that is, to the pure Sn corner.
Then, the solidification path changes to line (B), and
the primary phase that solidifies first becomes the
Sn phase. This is in good agreement with the SEM
observation in Fig. 8b and c, where the primary Sn
phase is observed in the solder after 10 min of
reflow. Since the solder composition changes with
increasing reflow time, that is, from Sn-9Zn to pure
Sn, the solder/CuZn5 interfacial energy might be
affected accordingly. Based on the morphological
evolution of the CuZn5 grain, the type of interfacial
energy is likely to be transformed from isotropic to
anisotropic.
It must be noted that, in Fig. 1, the Cu supply is
abundant, because the Cu substrate is thick. With
abundant Cu supply, the Cu-Zn compounds can
continuously grow by the reaction between Cu
and Zn. Thus, a significant change of the solder
C.-H. Chen, Lin, and C.-M. Chen
composition can occur, due to the continuous con-
sumption of Zn. In contrast, if the Cu supply is very
limited, for example, in the case using a thin Cu
substrate of only 4000 Å thickness (Fig. 6), the
consumption of Zn will be very limited. This might
merely result in a slight change of the solder com-
position, so the solidification behavior could be
described by line (A) in Fig. 9. This argument is
consistent with the results shown in Fig. 6, where
the primary Zn precipitates were formed near the
solder/CuZn5 interface. Owing to the negligible
change of solder composition, the solder/CuZn5
interfacial energy could remain isotropic. Therefore,
the CuZn5 grains on the 4000-Å Cu substrate
retained a rounded shape during reflow, as seen in
Fig. 7.
Effect of Cu Substrate Thickness
on the Reaction Products
Based on the experimental results, it can be seen
that, at the early stage of reflow, both CuZn5 and
Cu5Zn8 phases are formed, regardless of the fact
that the Cu substrate is only 4000 Å thin or as thick
as 0.5 mm. With increasing reflow time, the two
phases display different growth rates on different
Cu substrates. On the Cu substrates 6 lm, 10 lm,
and 0.5 mm thick (denoted as ‘‘thicker Cu’’ hereaf-
ter), the Cu5Zn8 phase grows dominantly, as seen in
Fig. 2. The dominant reaction product becomes
CuZn5 when the thickness of the Cu substrate is
reduced to 3 lm and 4000 Å (denoted as ‘‘thinner
Cu’’ hereafter). The results indicate that the type of
dominant reaction product in the Sn-9Zn/Cu inter-
facial reaction is significantly affected by the
thickness of the Cu substrate.
On the thicker Cu substrates, it is also found that,
although the CuZn5 phase is formed at the early
Effect of Cu Thickness on the Evolution of the Reaction Products at the Sn-9wt.%Zn Solder/Cu 65
Interface During Reflow

Fig. 4. Scanning electron micrographs of the solder/Cu interface

after reflow at 230°C for (a) 10 min and (b) 60 min, in which the
thickness of the Cu substrate is 10 lm.

Fig. 3. Top-view scanning electron micrographs of the reaction

compounds formed at the solder/Cu interface after reflow at 230°C Fig. 5. Scanning electron micrographs of the solder/Cu interface
for (a) 1 min, (b) 5 min, (c) 10 min, and (d) 60 min, in which the after reflow at 230°C for (a) 5 min and (b) 60 min, in which the
thickness of the Cu substrate is 0.5 mm. thickness of the Cu substrate is 3 lm.
66
Fig. 6. Scanning electron micrographs of the solder/Cu interface
after reflow at 230°C for (a) 1 min and (b) 10 min, in which the
thickness of the Cu substrate is 4000 Å.17
Fig. 7. Top-view scanning electron micrographs of the reaction
compounds formed at the solder/Cu interface after reflow at 230°C
for (a) 1 min and (b) 10 min, in which the thickness of the Cu sub-
strate is 4000 Å.
C.-H. Chen, Lin, and C.-M. Chen
Fig. 8. Scanning electron micrographs of lower magnification
showing the interior microstructure of the solder after reflow at 230°C
for (a) 5 min, (b) 10 min, and (c) 60 min, in which the thickness of the
Cu substrate is 0.5 mm.
stage of reflow, it disappears after a longer reflow
time. According to the Cu-Zn binary phase dia-
gram,19 the CuZn5 phase is thermodynamically
stable, so one interesting question arises as to why a
thermodynamically stable phase that has been
formed will disappear. To find a potential answer,
we use the isothermal section of the ternary Sn-Zn-Cu
system at 230°C20 in Fig. 10. In Fig. 10, it can be
seen that, at the Sn-rich corner, the liquid phase
(denoted as ‘‘L’’) can be in two-phase equilibrium
with the CuZn5, Cu5Zn8, CuZn, or Cu6Sn5 phases
with decreasing Zn concentration in the solder. At
the early stage of reflow, the Zn concentration in the
Effect of Cu Thickness on the Evolution of the Reaction Products at the Sn-9wt.%Zn Solder/Cu
Interface During Reflow
Fig. 9. Sn-rich region of the Sn-Zn binary phase diagram.19 Line (A)
is the solidification path of a hypo-eutectic SnZn alloy, line (B) is the
solidification path of a hyper-eutectic SnZn alloy, and L means liquid.
solder is still close to 9 wt.% (15.6 at.%, denoted as
‘‘a’’ in Fig. 10) as discussed above, so the interfacial
equilibrium can be represented by a tie-line in the
Fig. 10. Isothermal section of ternary Sn-Zn-Cu system at 230°C.20 Lines A and B are diffusion paths, L means liquid, a is the location of the
composition of Sn-9wt.% (15.6 at.%) Zn alloy, and b is that of SnZn alloy with Zn concentration less than 9 wt.%.
67
L + CuZn5 two-phase field. Therefore, CuZn5 can
form as a stable phase at the interface. The diffusion
path follows line A (thick dashed line) and is solder/
CuZn5/Cu5Zn8/Cu. However, the Zn concentration
will decrease with increasing reflow time (as indi-
cated by ‘‘b’’), due to the growth of the Cu-Zn com-
pounds. Thus, the interface status will shift toward
the Sn-rich tip. Then, the interfacial equilibrium is
represented by a tie-line in the L + Cu5Zn8 two-
phase field. The diffusion path becomes B (thin
dashed line) and is solder/Cu5Zn8/Cu. Therefore,
CuZn5 is no longer a stable phase and disappears, as
seen in Figs. 1d and 4b, leaving only Cu5Zn8 at the
interface. In contrast, for the thinner Cu substrates,
the change of the Zn concentration is insignificant,
as discussed above, so the interface status does not
change and can be still represented by a tie-line
in the L + CuZn5 two-phase field, remaining the
stability of CuZn5 at the interface.
Yang et al.21 reported the strong Zn concentration
effect on the interfacial reactions between Sn-Zn
solders and Cu substrates. They changed the Zn
concentration of the solder and found different
reaction products formed at the solder/Cu interface.
When the Zn concentrations were 0.5 wt.% and
2 wt.%, the reaction products were Cu6Sn5 and
Cu5Zn8, respectively. When the Zn concentration
was in-between (0.7 wt.%), Cu6Sn5 and CuZn coexis-
ted. Yang et al. also provided an explicit explana-
tion of the strong Zn concentration effect, using the
ternary Sn-Zn-Cu isothermal section. Based on
68
their results and those obtained in our work, it can
be expected that Cu5Zn8 can form as a stable phase
at the Sn-Zn solder/Cu interface when the Zn con-
centration in the solder is in the range from 2 wt.%
to 9 wt.%. However, the CuZn5 phase was not
observed in their results, indicating that CuZn5 is,
indeed, not a thermodynamically stable phase for
the solder with lower Zn concentration, which is in
agreement with the above discussion of Figs. 1d and
4b.
Estimation of Densities of Cu5Zn8 and CuZn5
The density of the intermetallic compounds is a
fundamental physical parameter which is useful in
many applications. However, the relevant informa-
tion is very limited, and no data on the densities of
the Cu-Zn compounds can be obtained. In our work
described here, the densities of the Cu-Zn com-
pounds could be estimated preliminarily from the
thickness data of the Cu-Zn compounds. For exam-
ple, as seen in Fig. 4, the Cu substrate had been
completely consumed and transformed into the
Cu5Zn8 phase at the interface after reflow for
60 min. If the Cu solubility in the solder is assumed
to be negligible, all of the Cu atoms participate in
the interfacial reaction with Zn via the following
chemical reaction.
5Cu þ 8Zn ! Cu5 Zn8 (1)
Since the Cu substrate is 10 lm thick, it can provide
(dCu 9 DxCu 9 A)/MCu = 1.41 9 10-12 9 A mol of Cu
for the interfacial reaction, where dCu is the density
of Cu (8.96 g/cm3), DxCu is the thickness of the Cu
substrate (10 lm), A is the contact area between
solder and Cu, and MCu is the molecular weight of Cu
(63.54 g/mol). According to reaction (1), 1 mol of Cu
can produce 0.2 mol of Cu5Zn8. Therefore, from the
parameters MCu5 Zn8 (840.82 g/mol) and DxCu5 Zn8
(21.88 lm) obtained from Fig. 2, the density of the
Cu5Zn8 phase is estimated to be 10.84 g/cm3. The
density of the CuZn5 phase can also be obtained from
the results of the 4000 Å Cu substrate. Based on the
chemical reaction shown below, the CuZn5 density is
estimated to be 7.64 g/cm3.
Cu þ 5Zn ! CuZn5 (2)
It must be mentioned that the above estimation is
very simplified, since several uncertainties that
may cause errors of the estimation are ignored.
These uncertainties come from the measurement of
the compound thickness, the assumption of negli-
gible Cu solubility in the solder, etc. While the
estimated results should be valuable for pre-
liminary reference since no data can be obtained
currently, more accurate measurements have to be
conducted to confirm further their accuracy.
C.-H. Chen, Lin, and C.-M. Chen
CONCLUSIONS
Two compounds, CuZn5 and Cu5Zn8, were formed
at the solder/Cu interfaces reflowed at 230°C for Cu
substrates ranging in thickness from 4000 Å to
0.5 mm. However, the evolution of the two
compounds during reflow was affected significantly
by the thickness of the Cu substrate. When the Cu
substrate was thicker than 6 lm, CuZn5 disappeared
but Cu5Zn8 kept on growing after a longer reflow
time, while, as the Cu thickness was reduced to fewer
than 3 lm, Cu5Zn8 shrank with increasing reflow
time but CuZn5 grew dominantly. The thickness of
the Cu substrate also had noticeable effects on the
evolution of the CuZn5 grain structure. With
increasing reflow time, the CuZn5 grains retained a
rounded shape on thinner Cu substrates; however,
the CuZn5 grains became faceted and displayed
preferential growth orientations on the thicker Cu
substrates. This noticeable effect was ascribed to the
change of the solder composition due to the Cu/Zn
interfacial reaction. The phase evolution can be
explained by the ternary Sn-Zn-Cu phase diagram.
ACKNOWLEDGEMENTS
The authors wish to acknowledge the financial
support of the National Science Council of Taiwan,
ROC, through Grants NSC 95-2221-E-005-143 and
NSC 96-2218-E-007-012. This work was supported
in part by the Ministry of Education, Taiwan, ROC,
under the ATU plan.
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