Introduction

Concerns about the health and envi-

ronmental hazards of lead, and legislative
actions around the world drove the re-
search community to find replaceable sol-
der alloys for the traditional Sn-Pb alloys
(Refs. 13). Among the lead-free candi-
dates that have been developed, such as
Sn-Ag, Sn-Cu, Sn-Bi and Sn-Zn alloy sys-
tems, Sn-Zn alloy has been receiving spe-
cial attention due to its low cost, wide raw
material sources, superior strength, and
low melting point near to eutectic Sn-Pb
solder (Ref. 4). Nevertheless, there are
still several problems that need to be ad-
dressed in order to facilitate the practical
use of this solder alloy, such as its inferior
wettability and easy oxidation (Refs. 5, 6).
Heretofore, a lot of research has been
done to improve the performances of the
Sn-Zn solders (Refs. 68). Recent studies
also pointed out that Sn-Zn-Ag-Ga-Al-Ce
alloy presented good solderability and an-
tioxidiation (Refs. 9, 10). These efforts are
expected to promote the use of Zn-con-
taining lead-free solders in the electronics
industry.
Solders are typically melted on a metal-
lic substrate, such as Cu or Ni. Formation
of intermetallic compounds (IMCs) is es-
sential in the manufacturing (Refs. 11, 12).
IMCs formed at the interface are a pre-
requisite for good solderability. It is re-
ported that interfacial reaction may be a
dominant factor in promoting the wetting,
compared with the side effect of surface
roughness (Ref. 13). Moreover, IMCs
formed at the interface also have a signif-
icant effect on the mechanical properties
and reliability of the soldered joints (Refs.
14, 15). This is because the brittle nature
of the IMCs and the joining of the two ma-
terials with dissimilar properties, such as
thermal expansion coefficient, hardness,
and Youngs modulus, would degrade the
interface integrity between solder and sub-
strate (Ref. 14). Thus, a comprehensive
knowledge of the intermetallic phases
formed at the interface and its mechanical
properties is extremely important.
It is known that Cu-Zn intermetallic
compounds form between Sn-Zn solders
and Cu substrate (Ref. 16); however, the
reaction products may change when other
elements are added to the solder or vari-
ous substrates are used (Refs. 15, 17). In
the literature, most of the studies were
carried out to find the mechanical proper-
ties of the Cu-Sn, Ni-Sn, and Cu-Ni-Sn
based intermetallics that are associated
with Sn-Pb, Sn-Ag, and Sn-Ag-Cu solders
(Refs. 12, 1821). However, to the best of
our knowledge, the micromechanical
property data for the IMCs associated
with Sn-Zn solders and different sub-
strates were rarely reported in the litera-
ture survey conducted. The aim of this
study is to investigate the solderability and
the intermetallic compounds formed be-
tween Sn-9Zn-0.25Ag-0.2Ga-0.002Al-
0.15Ce solder and three types of widely
utilized substrates: Cu, Au/Ni/Cu, and Sn-
plated Cu.
Experimental Procedures
Material Preparation
Pure Sn, Zn, Ag, Al, Ga, and Ce
(99.95% pure) were used in the present in-
vestigation. The raw materials were first
melted in a ceramic crucible to prepare Sn-
9Zn, Sn-9Zn-0.1Al, Sn-9Zn-1Ag, Sn-9Zn-
2Ga, and Sn-9Zn-4Ce as master alloys. In
SUPPLEMENT TO THE WELDING JOURNAL, DECEMBER 2010
Sponsored by the American Welding Society and the Welding Research Council
Investigations of Sn-9Zn-Ag-Ga-Al-Ce Solder
Wetted on Cu, Au/Ni/Cu, and Sn-plated Cu
Substrates
The solderability of Zn-containing, lead-free alloys was examined to determine
whether they are good candidates for use in the electronics industry
BY H. WANG, S. XUE, W. CHEN, X. LIU, AND J. PAN
KEYWORDS
Lead-Free Solder
Sn-Zn
Solderability
Nanoindentation
Interfacial Reaction
Intermetallic Compounds
H. WANG is with faculty of Materials Science &
Chemical Engineering, Ningbo University, and
the College of Materials Science and Technology,
Nanjing University of Aeronautics and Astronau-
tics, P.R. China. S. XUE and W. CHEN are with
College of Materials Science and Technology,
Nanjiing University of Aeronautics andAstronau-
tics, P. R. China. X. LIU and J. PAN are with fac-
ulty of Materials Science & Chemical Engineer-
ing, Ningbo University, P. R. China.
ABSTRACT
Interfacial reaction products between Sn-9Zn-0.25Ag-0.2Ga-0.002Al-0.15Ce solder
and Cu, Au/Ni/Cu, Sn-plated Cu substrates were investigated by scanning electron mi-
croscope (SEM) and X-ray diffraction (XRD), while the hardness and indentation mod-
ulus of the interface reaction products were studied by the nanoindentation technique
(NIT). The SEM and XRD results indicated that interfacial reaction products between
solder and substrates were Cu
5
Zn
8
, AgZn
3
, AuZn
3
, and Ni
5
ZSn
21
. A Cu
5
Zn
8
/ Sn/
Cu
5
Zn
8
sandwich structure formed at the interface between solder and Sn-plated sub-
strate. The hardness and modulus values of Cu
5
Zn
8
and Ni
5
Zn
21
obtained through NIT
were noticeably high, while that of Sn-9Zn-0.25Ag-0.2Ga-0.002Al-0.15Ce solder was
low, exhibiting significant plasticity. Moreover, the wetting balance test and mechanical
property test indicated that Sn-9Zn-0.25Ag-0.2Ga-0.002Al-0.15Ce solder exhibited good
solderability on Sn-plated Cu substrate, and the application of Au/Ni/Cu substrate may
enhance the soldered joints.
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the melting process, KCl+ LiCl molten salt,
with the mass ratio of 1.3:1, was used over
the surface of the liquid alloys to prevent
oxidation during smelting. Then the exper-
imental alloys were melted in a quartz cru-
cible at 300C by using the master alloys. In
order to avoid oxidation and ensure the ac-
tual compositions of the alloy elements
match the designed value, the entire melt-
ing process was carried out in a nitrogen at-
mosphere. Finally, the contents of Zn, Ag,
Ga Al, and Ce in the alloy were tested by
the inductively coupled plasma auger elec-
tron spectroscopy (ICP-AES) method. The
result is shown in Table 1.
Pure Cu, Au/Ni/Cu, and Sn-plated/Cu
flakes, respectively, were employed as wet-
ted substrates.The Au/Ni/Cu flakes were
constructed by electroplating Au/Ni over
underlying Cu flakes, while the Sn-
plated/Cu flakes were
electroplated Sn on Cu
substrate. The size of
test flakes was 0.3 5
30 mm.
The quad flat pack-
age (QFP) device with
48 leads (the size of the
QFP leads was 0.2
0.5 mm) and ceramic
resistors (CR)(the size
of the CR pad is 1.25
0.5 mm) were sol-
dered on FR-4 printed
circuit boards (PCB).
The pads of PCB are
made of Cu, Sn-plated/
Cu, and Au/Ni/Cu,
respectively.
Wetting Balance Test
Wetting experiments were performed
by a SAT-5100 wetting tester (Rhesca Co.
Ltd., Japan) according to Japanese Indus-
try Standard JIS Z 3198-4, Test methods for
lead-free solders Part 4: Methods for sol-
derability test by a wetting balance method
and a contact angle method. Figure 1 shows
a typical wetting curve in the wetting bal-
ance test. According to Fig. 1, the molten
solder climbs up on the sample flake (e.g.,
Cu) due to the wetting force exerted on it
when it is dipped into the solder bath. This
is similar to the situation in wave solder-
ing, where a wave of molten solder is
brought into contact with the substrate.
Wetting that occurs in a short time (t
0
)
with a high peak wetting force (F
max
) is
considered to be good.
The wetting balance test was per-
formed at 235C in air atmosphere applied
with middle active rosin (MAR) flux. Pure
Cu, Au/Ni/Cu, and Sn-plated/Cu flakes
were employed as substrates. The flakes
were immersed into the molten solder for
10 s, and the immersion depth was 2 mm.
Microstructure of the Interface
In order to investigate the reaction
products on the interface, pure Cu,
Au/Ni/Cu, and Sn-plated/Cu substrates
were dipped in Sn-9Zn-0.2Ga-0.002Al-
0.25Ag-0.15Ce solder for 30 s at 235C to
achieve reaction layers. After that, some
of the wetted flakes were cross sectioned
for scanning electronic microscope (SEM)
analysis, and the other dipped substrates
were immersed into a solution, 99%
CH
3
OH + 0.5% HCl + 0.5% HNO
3
, to
remove the unreacted solder. Then the ex-
posed IMCs were further characterized by
X-ray diffraction (XRD).
Nanoindentation Test
The nanoindentation technique ex-
plored in this work is an attractive tech-
nique for extracting Youngs modulus of
the IMCs because of the relatively small
volume tested. Indeed, the properties
measured from nanoindentation are the
true properties of the IMC layer.
A nanoindenter SHIMADZU DUH-
W201S equipped with a Berkovich 115-deg
diamond-probe tip, three-sided pyramidal
indenter was employed. After the area of in-
terest was focused, the nanoindentation test
was conducted under a 50-mN load. The
loading and unloading rates were both 2
mN/s and held at 50 mN for 10 s.
In order to achieve thick IMC layers,
the substrates were first dipped into the
molten solder for 10 min at 260C, and
then annealed at 150C for 300 h, so that
at least 20 m IMC layers would form.
Thus, the size of the IMC layers in these
joints was sufficient to be analyzed for the
nanoindentation test. After the test, an op-
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Table 1 Chemical Composition of the Prepared Solder (wt-%)
Element Zn Ag Ga Al Ce Sn
Content 8.895 0.194 0.197 0.002 0.135 Balance
Fig. 1 Wetting curve in the wetting balance test.
xFig. 3 Solderability of Sn-9Zn-0.2Ga-0.002Al-0.25Ag-0.15Ce solder
wetted on different substrates.
Fig. 2 Schematic illustrations of the mechanical property test of micro-
joints.
Wang -- 12-10:Layout 1 11/10/10 2:37 PM Page 250
tical microscopy was employed to identify
the indentation traces. The mechanical
properties were obtained by averaging five
experimental indents, which were selected
by optical microscopy to avoid the bound-
ary effects. All the tests were carried out
out at 20C.
Mechanical Property Tests
In order to reflect the actual instances
in the electronic assembly industry, the
mechanical property tests of the micro
joints were carried on according to Japan-
ese Industry Standard JIS Z 3198-6, Test
methods for lead-free solders Part 6:
Methods for 45-deg pull test of solder joints
on QFP lead, and Part 7: Methods for shear
test of solder joints on chip components,
with an STR-1000 joint strength tester, as
schematically shown in Fig. 2.
First, the flat packages and ceramic re-
sistors were soldered on PCB by Sn-9Zn-
0.2Ga-0.002Al-0.25Ag-0.15Ce solder at
250C. Subsequently, the pull and shear
tests of the soldered joints were carried
out at room temperature. The pull speed
and shear speed were set as 2 and
10mm/min, respectively.
Results and Discussions
Solderability of Solder
Figure 3 shows the solderability of the
solder wetted on different substrates. It is
found that the solder exhibits better solder-
ability on Sn-plated/Cu substrate, with
higher wetting force and shorter wetting
time, than on Au/Ni/Cu substrates. The wet-
ting time using Cu substrate and Sn-plated
Cu substrate are similar; however, the F
max
on the Sn-plated Cu is higher than that on
the Cu substrate. The higher F
max
may be
attributed to the Sn-plated layer, which can
reduce the interfacial tension between sol-
der and substrate. It is reported that Sn-
plated pads can improve the solderability of
Sn-Ag-Cu and Sn-Cu solders (Ref. 22). The
results shown in Fig. 3 also indicated that
the Sn-plated/Cu substrate can improve the
solderability of Zn-bearing solder.
Interfacial Reactions between the Solder
and Substrates
Figure 4 shows the backscattering elec-
tron image associated with EDS and XRD
analysis of the interface between Sn-9Zn-
0.2Ga-0.002Al-0.25Ag-0.15Ce solder and
Cu substrate. According to Fig. 4A, it is no-
table that the interfacial IMCs can be clearly
divided into two portions, a planar layer,
and an additional scallop-like layer. Ac-
cording to the EDS analysis, the planar one
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A
A
B
B C
Fig. 4 A Interface between Sn-9Zn-0.2Ga-0.002Al-0.25Ag-0.15Ce solder and Cu substrate; B XRD pattern of IMCs.
Fig. 5 A Interface between Sn-9Zn-0.2Ga-0.002Al-0.25Ag-0.15Ce solder and Sn-plated Cu substrate; B EDS scanning along the IMC layer; C XRD
pattern of the IMCs.
Table 2 Indentation Modulus and Hardness of the Materials Tested
Material Indentation Modulus (GPa) Hardness (GPa)
Cu
5
Zn
8
162.1 8.6 4.92 0.50
Ni
5
Zn
21
159.3 7.2 5.12 0.52
AgZn
3
124.4 2.5 3.52 0.21
AuZn
3
118.2 2.2 3.40 0.20
Cu 115.7 1.2 1.70 0.36
Solder 59.9 3.2 0.36 0.07
Wang -- 12-10:Layout 1 11/10/10 2:37 PM Page 251
is mainly composed of Cu and Zn, while the
scallop-like one contains much more Ag.
The XRD pattern shown in Fig. 4B indi-
cates that these IMCs are Cu
5
Zn
8
and
AgZn
3
. The formation of AgZn
3
is consid-
ered that, due to the formation of Cu
5
Zn
8
,
zinc atoms transfer from the liquid solder to
the substrate and enrich at the interface.
Meanwhile, silver atoms also segregate at
the interface and react with zinc to form
Ag
5
Zn
8
. The Gibbs free energy
of Ag
5
Zn
8
is smaller than that
of AgZn
3
and AgZn IMCs at
235C (Ref. 23) by heteroge-
neous nucleation on the pre-
formed Cu
5
Zn
8
interface, since
Cu
5
Zn
8
and Ag
5
Zn
8
exhibit
identical structure and their lat-
tice constants do not differ
greatly. Furthermore, the sub-
sequent peritectic reaction: L +
-Ag
5
Zn
8
AgZn
3
con-
tribute to the AgZn
3
observed
at the interface (Ref. 24).
Figure 5 shows the in-
terface between the solder and
Sn-plated/Cu substrate, associ-
ated with the line scanning and
XRD pattern of the IMC
layer. The XRD pattern indi-
cated that the IMC is Cu
5
Zn
8
.
According to the line scanning,
a thin Sn layer still exists in the
middle of the Cu
5
Zn
8
layers, forming a
sandwich structure. The formation of the
sandwich structure is mainly because that,
during the wetting period, Zn atoms dif-
fuse through the Sn layer and then react
with Cu atoms, while the Cu atoms also
diffuse through the Sn layer to the molten
solder and react with Zn atoms to form
Cu
5
Zn
8
. At the same time, the Sn layer
may melt to the molten sol-
der as the wetting tempera-
ture is 235C, a little higher
than the melting point of
Sn. Before the substrate
was taken out of the solder,
the Sn layer had not melt
completely, as a result the
aforementioned sandwich
structure formed.
Figure 6 shows the
backscattering electron
image of the interface be-
tween the solder and
Au/Ni/Cu substrate, associ-
ated with the EDS and XRD
analysis of the IMCs layer.
The XRD pattern shown in
Fig. 6C indicates that the
IMCs are AuZn
3
and a little
AuAgZn
2
. However, the Ni
layer and the Ni-Zn IMCs
layer were covered by the
AuZn
3
and the remnants
solder, thus they were not
detected by the XRD analy-
sis. The EDS indicated that
the Ni layer was composed
of Ni and Zn, according to
the report in Ref. 17. We
supposed that this layer was
Ni
5
Zn
21
.
Indentation Test
The indentation test
was carried out on both Sn-9Zn-0.25Ag-
0.2Ga-0.002Al-0.15Ce solder, Cu sub-
strate, and the four IMCs: Cu
5
Zn
8
,
AgZn
3
, AuZn
3
and Ni
5
Zn
21
. Figure 7
shows the indentation traces on different
materials tested. However, a thick AgZn
3
layer can be hardly achieved, according to
the report in Ref. 22, massive AgZn
3
ex-
ists in Sn-9Zn-2Ag solder, and thus the in-
dentation test on AgZn
3
phase was carried
on Sn-9Zn-2Ag solder as shown in Fig.
7D. According to Fig. 7, it is found that the
indentation trace in the IMCs is smaller
than that in the solder. This is because that
the IMCs are much harder than the solder.
Figure 8 shows the load-displacement
plots obtained by the load indentations per-
formed on the aforementioned materials.
From the load-displacement curves, a hard-
ness and elastic modulus are measured that
are useful in describing the deformation be-
havior of the solder and IMCs.
Analysis of load-displacement data was
carried out according to the Oliver and
Pharr method (Refs. 24, 25). At the maxi-
mum load, P
max
and hardness, H
NI
is de-
termined by H
NI
= P
max
/ A(h
c
), where
A(h
c
) is the projected contact area. From
the slope of the unloading curve, a re-
duced modulus E
r
is measured that ac-
counts for elastic recovery of the sample
and the indenter:
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Fig. 6 A Interface between Sn-9Zn-0.2Ga-0.002Al-0.25A-
0.15Ce solder and Au/Ni/Cu substrate; B EDS analysis of point
A; C EDS analysis of point B; D EDS analysis of point C;
E XRD pattern of the IMCs.
A B
C
D
E
Wang -- 12-10:Layout 1 11/10/10 2:38 PM Page 252
where E is the Youngs modulus and is
Poissons ratio. With the properties of the
diamond indenter known (E = 1140 GPa,
and = 0.07), the indentation modulus,
E
NI
, is defined as E
NI
= E/1
2
|
sample
.
Indentation modulus is primarily what will
be reported here; however, with knowl-
edge of Poissons ratio of the test material,
the Youngs modulus, E, can be
determined.
Table 2 shows the results calculated ac-
cording to the data in Fig. 8. In examining
the results obtained, the maximum pene-
tration of the indenter for Sn-9Zn-0.25Ag-
0.2Ga-0.002Al-0.15Ce solder is
approximately four times that measured for
Cu
5
Zn
8
. The solder is found to be very soft,
with a hardness of 0.36 GPa, exhibiting sig-
nificant plasticity. In contrast to the solder,
the IMCs, Cu
5
Zn
8
, and Ni
5
Zn
21
, are signif-
icantly harder while the hardness of AgZn
3
and AuZn
3
is similar to that of Cu. The in-
termetallic compound had a higher modu-
lus than either of the two components. The
higher modulus of the intermetallic over
that of either of the metallic components
E
E E
r sample indenter
=

+

1 1
2 2
1

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B
C D
E
Fig. 7 Indentation traces on the following: A Cu
5
Zn
8
; B Ni
5
Zn
21
;
C AuZn
3
; D AgZn
3
; E solder.
Fig. 8 Plots of load vs. depth for 50-mN maximum load indentations per-
formed on Cu, solder, and IMCs.
Wang -- 12-10:Layout 1 11/10/10 2:39 PM Page 253
can be attributed to the combination of
ionic/covalent bonding in intermetallic com-
pounds, which may result in a higher mod-
ulus than that obtained from a simple rule
of mixtures of the components (Ref. 26). It
should be noted that although AgZn
3
and
AuZn
3
are intermetallic compounds, they
do exhibit some extent of plasticity.
Hardness is often used to explain the
brittleness of a material. The indication is
that Cu
5
Zn
8
and Ni
5
Zn
21
have the poten-
tial for brittle behavior (crack initiation)
when the soldered joints were deformed by
stress. AgZn
3
and AuZn
3
, with a lower
hardness and modulus, are actually rather
soft and ductile and not a likely source of
crack initiation. Actually, cracks were found
located at the Cu
5
Zn
8
layer, and the inter-
face between AuZn
3
and Ni
5
Zn
21
layer, as
shown in Fig. 9.
Mechanical Properties of Soldered Joints
Figure 10 shows the results of the me-
chanical properties of the QFP and CR mi-
crojoints. According to Fig. 10, it is found
that the joints on the Au/Ni/Cu substrate ex-
hibit higher shear and
pull force than that on
the Cu substrate, while
the joints on the Sn-
plated/Cu substrate
show lower shear and
pull force than that on
the Cu substrate.
It is known that Sn (Zn
for Sn-Zn solders) at the
solder/Cu interface re-
acts rapidly with Cu to
form Cu-Sn (Cu-Zn for
Sn-Zn solders) IMCs,
which weaken the sol-
dered joints (Refs.
2425). Therefore, Ni is
used as a diffusion bar-
rier layer to prevent the
rapid interfacial reac-
tions between the solder and Cu layer in
electronic devices. In this study, it was found
that the application of Au/Ni/Cu substrate
can really enhance the soldered joints. It
was also found that Sn-plated/Cu substrate
can improve the solderability however, it
may deteriorate the soldered joints.
Conclusions
1) Sn-9Zn-0.25Ag-0.2Ga-0.002Al-0.15
Ce solder shows better solderability on Sn-
plated Cu substrate than that of pure Cu
and Au/Ni/Cu; while the application of
Au/Ni/Cu pads may deteriorate the sol-
derability. A mechanical property test in-
dicated that the application of Au/Ni/Cu
substrate enhanced the soldered joints.
2) Cu
5
Zn
8
and AgZn
3
intermetallic
compounds form at the interface between
Sn-9Zn-0.2Ga-0.002Al-0.25Ag-0.15Ce sol-
der and Cu substrate, while AuZn
3
and
AuAgZn
2
were present at the interface be-
tween the solder and Au/Ni/Cu substrate.
When the Sn-plated Cu substrate was used,
the Cu
5
Zn
8
layers and the remnants Sn
layer constituted a sandwich structure at the
interface.
3) Cu
5
Zn
8
and Ni
5
Zn
21
may be the
crack initiation point when the soldered
joint was deformed by stress due to the
high hardness and modules. On the other
hand, Sn-9Zn-0.25Ag-0.2Ga-0.002Al-
0.15Ce solder is soft and exhibits signifi-
cant plasticity, while AgZn
3
and AuZn
3
also exhibit a little plasticity.
Acknowledgments
The paper was sponsored by the K.C.
Wang MagnaFund, Ningbo University. The
authors would also like to acknowledge the
support from the Talent Project Fund (019-
B00228104700), and Dr. Jun Huang for the
nanoindentation measurements.
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255-s WELDING JOURNAL
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