Materials Science & Engineering A 669 (2016) 403–416

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Effect of Ni and Sb additions and testing conditions on the mechanical

properties and microstructures of lead-free solder joints
Q.B. Tao a, L. Benabou a,n, L. Vivet b, V.N. Le a, F.B. Ouezdou a
a
LISV, Université de Versailles Saint-Quentin-en-Yvelines, Paris Saclay University, France
b
Valeo GEEDS Laboratory, 78321 La Verriere, France

art ic l e i nf o a b s t r a c t

Article history: Nowadays, one of the strategies to improve the reliability of lead-free solder joints is to add minor
Received 13 April 2016 alloying elements to solders. Therefore, the aims of this study are to investigate the effect of Ni and Sb, as
Received in revised form well as that of the testing conditions (temperature and strain rate), on the mechanical properties of two
24 May 2016
new lead-free solder joints, Sn-3.8Ag-0.7Cu-3Bi/Cu and Sn-3.8Ag-0.7Cu-3Bi0.2Ni1.54Sb/Cu. The changes,
Accepted 25 May 2016
after testing, in their respective microstructure will also be investigated. The procedure to fabricate
Available online 26 May 2016
appropriate joint samples is described in this research. The shear tests were conducted by micro-tensile
Keywords: machine at temperatures between room temperature and 125 °C and strain rates between 2.0
10  4 s  1
Pb-free solder and 2.0
10  2 s  1. The experimental results indicate that, with additions of Ni and Sb in Sn-3.8Ag-
Alloy element
0.7Cu-3Bi, the ultimate tensile strength (UTS) and the yield stress ( σy ) are improved. Moreover, both
Mechanical characterization
temperature and strain rate may have substantial effects on the mechanical behavior and the micro-
Deformation and fracture
Intermetallics structural features of the solder alloys. During the shear tests, the strength decreases with the increase of
Finite element method the test temperature and/or the decrease of the strain rate. The enhanced strength is attributed to the
solid solution hardening effects of Sb in the Sn matrix and the refinement of the microstructure with the
addition of Ni. Ni and Sb additions lead to the formation of new (Cu, Ni)6Sn5 and Ag3(Sn, Sb) IMCs.
Needle-like (Cu, Ni)6Sn5 appeared in the Sn-3.8Ag-0.7Cu-3Bi0.2Ni1.54Sb/Cu, instead of the globular-like
Cu6Sn5 inSn-3.8Ag-0.7Cu-3Bi/Cu. In addition, the nine Anand material parameters are identified using
the shear stress-strain data and a non-linear least square fitting and its validity is checked by means of
the experimental data. The findings found that these Anand parameters are also in good agreement with
data given in literature for other solder alloys. The obtained material parameters of the Anand con-
stitutive model were utilized to analyze the stress-strain response of an Insulated Gate Bipolar Transistor
(IGBT) under thermal cycling. Furthermore, the SEM analysis of as-fabricated joint specimens as well as
fractured specimens at different testing conditions was done to observe the effects of these factors on the
microstructure of the solder alloys.
& 2016 Elsevier B.V. All rights reserved.

1. Introduction their advantages of good wetting property, superior interfacial

In the past few decades, tin-lead solders have been widely used
as a primary solder material in the electronic industry. However,
the concern over the toxic effect of lead in eutectic Sn-Pb solders
on both human health and the environment has prompted the
development of lead-free solder alloys in electronic packaging [1].
Furthermore, some governments have published laws banning the
use of tin-lead solders in electronic packaging. Hence, manu-
facturers have been pursuing a new generation of lead-free solders
to replace tin-lead solders. Undoubtedly, they are the most pro-
mising Pb-free replacements for conventional Sn-Pb solders due to
n
Corresponding author.
E-mail address: lahouari.benabou@uvsq.fr (L. Benabou).
properties, high creep resistance and low coarsening rate [2,3]. The
most popular candidates for replacement of the lead-containing
solder alloys are Sn-Ag-Cu (SAC), Sn-Cu, Sn-Ag, Sn-Zn, etc. solders.
Although the melting temperature is higher and the wettability
poorer than conventional Sn-Pb eutectic solder, they have better
mechanical properties [4–7]. Therefore, Sn-Ag alloys are expected
to be the substitute for Sn-Pb eutectic solder. While Sn-Cu solder is
considered the candidate alloy to replace eutectic Sn-Pb solder for
wave soldering [8,9], SAC305 and SAC387 alloys are considered
lead-free standard alloys for electronic assemblies because they
have good mechanical properties and wettability [10,11]. However,
there are still some drawbacks associated with these alloys [12,13].
For example, SnAg3.5 and SnCu0.7 have very high processing
temperatures and limited reliability in high operation temperature
applications. SnAg3.8Cu0.7 also has limited reliability in high

http://dx.doi.org/10.1016/j.msea.2016.05.102
0921-5093/& 2016 Elsevier B.V. All rights reserved.
404 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416
operation temperature applications.
In order to improve the properties of these lead-free solders,
some alloying elements have been added to the lead-free solders.
Among the alloying elements, the most popular choice are Ni, Bi,
Sb, Mn, Ti, Ce and Co. They are used to generate new solders which
can be used in some demanded services. While Sb addition in-
creases the liquidus temperatures, shear strength and creep re-
sistance [14–16], Ni addition enhances creep resistance due to
formation of intermetallic phases [17,18]. Bi addition increases
hardening and creep resistance but decrease melting temperature
[19]. On the other hand, some elements are rejected from the alloy
because of some disadvantages such as In increases cost and slight
toxicity, Cs is toxic, and Te is highly toxic and increases melting
temperature [20]. Other alloying elements can reduce the melting
temperature of the lead-free solders while concurrently improving
its mechanical properties [21–24]. Studies’ results have confirmed
that the new solders, which contain Sb and Bi, provide higher
reliability under high operating temperatures and high stress
conditions. Among the newly-developed solder alloys,
Sn3.8Ag0.7Cu-3Bi and Sn3.8Ag0.7Cu-3Bi0.2Ni1.54Sb (hereinafter
termed SAC-Bi and INNOLOT, respectively) are chosen as the ma-
terial for interconnection in electronic packaging for the auto-
motive industry.
Up to date, with increasing requirements for smaller, less ex-
pensive, longer life expectancy and lead-free electronic devices, it is
desirable to know how solder joints behave mechanically in elec-
tronic packaging. Furthermore, it is well-known that solder joints in
electronic devices experience a wide range of strain rates and
temperatures, and so it is important to understand how the me-
chanical behavior of solder alloys varies with changes in these
factors. For example, automotive electronics manufacturers are fa-
cing significant challenges in respect to the thermo-mechanical
reliability of solder joints. Solder joints display a much more com-
plex structure than a bulk material. In general, for reliability analysis
of solder joints, tensile and shear tests are conducted to investigate
the mechanical properties of lead-free solders. For tensile tests,
dog-bone and flat type specimens with different dimensions were
used. On the other hand, lap shear joint type specimens that have
the same thickness as in real packaging were used to evaluate the
shearing behavior of the solders. Some previous studies have al-
ready focused on the mechanical behavior of bulk and joint solders
[2,25–29]. The tensile and shear properties of such SAC based lead-
free solder alloys were reported in many studies [30–33]. Re-
searches on the effects of strain rate and temperature on the me-
chanical properties have been done on solders [28,34–38]. Also,
some studies have focused on the effect of alloy additions in the
microstructure and on the mechanical behavior of solder joints
[3,15,17,18,31,39,40]. However, a literature review revealed that no
known studies have been reported so far on the simultaneous effect
of Ni and Sb and testing conditions on the mechanical properties
and microstructure of the SAC-Bi solder joint.
In this paper, two novel solder alloys, namely SAC-Bi and IN-
NOLOT, which have begun to come into use in the electronic
packaging, were used to fabricate lap shear joint specimens. A
large number of shear tests were conducted at various strain rates
ranging from 2.0
10  4 s  1 to 2.0
10  2 s  1 over a wide range of
temperature - from room temperature to 125 °C - for comparison.
Table 1.
Chemical compositions of the solder alloys (mass %), and the solidus and liquidus temperatures.
Solders Sn Ag Sb Cu Bi
INNOLOT Bal. 3.80 1.54 0.70 3.00
SAC-Bi Bal. 3.80 o0.001 0.70 3.00
SAC387 Bal. 3.80 o0.001 0.70 o 0.0016
The purpose of these tests is to investigate in a systematic manner
the effect of Ni and Sb atoms and testing conditions (strain rate
and temperature) on the material properties of the solder alloys as
data on the mechanical properties of these newly-developed lead-
free solder alloys is still lacking. It turned out that the UTS and σy
of the two solders which had been added Ni and Sb atoms were
improved. With more Sb and Ni addition, the INNOLOT solder has
better shear strength than the SAC-Bi solder at the same strain
level and testing temperature. In addition, the experimental data
was used to identify the material parameters of the viscoplastic
constitutive law of Anand using a non-linear least square fitting
method and then a FEM simulation, based on the obtained Anand
parameters, was performed to analyze the stress-strain response
of an Insulated Gate Bipolar Transistor (IGBT) under thermal cy-
cling. Eventually, the microstructures of some selected as-fabri-
cated and broken test specimens were analyzed by the use of a
scanning electron microscope (SEM) to study the microstructure
and fracture surface of the samples.
2. Experimental procedures
2.1. Materials
The Sn3.8Ag0.7Cu-Bi3.0 (SAC-Bi) and Sn3.8Ag0.7Cu-Bi3.0-
Ni0.2Sb1.54 (INNOLOT) solder alloys were used in this study. The
chemical composition and the solidus and liquidus temperatures
of the two solder alloys compared with Sn3.8Ag0.7Cu (SAC387)
lead-free solder are shown in Table 1. It is obvious that the SAC-Bi
and INNOLOT solders were made by introducing minor additions
of Bismuth (Bi), Nickel (Ni) and Antimony (Sb) elements to SAC387
solder. However, the amount of these alloys added in the INNOLOT
is much more than that in the SAC-Bi, 1.54 wt% compared with
0.001 wt% of Sb and 0.2 wt% compared with 0.001 wt% of Ni in the
INNOLOT and SAC-Bi, respectively. The effect of these addition
alloys on the mechanical behavior and the microstructure char-
acteristics will be discussed in the next sections.
2.2. Sample preparation
The lap-shear technique has been widely used to evaluate
shear, creep and thermal fatigue behavior of solder joints for dif-
ferent solder alloys. In this study, we proposed a method to fab-
ricate miniature single lap-shear joint specimens with dimensions
that represent the actual solder joints used in the automotive and
microelectronic devices. The procedure for fabricating lap-shear
joint specimens is done as follows:
(1) A lap shear specimen is prepared by soldering two copper (Cu)
substrates using the SAC-Bi or INNOLOT solder preform of 0.20
mm thickness. The Cu substrates are previously cut with
electrical discharge machining according to a specific geo-
metry, and then the surfaces for soldering are ground and
polished using SiC papers. The impurities on the Cu substrates
are removed by dipping them into 50% nitric acid for 20 s and
then quickly in acetone;
Fe Al As Ni Liquidus (C) Solidus (C)
0.003 o 0.001 0.005 0.2 218 206
0.0015 o 0.001 0.005 o0.001 226 221
0.0005 0.0005 0.0008 o0.0002 217 220
 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416 405

(2) (ii) After air drying, solder flux is dispersed on the polished
area to enhance wetting when the solder sheet is applied;
(3) The solder sheet, cut with the right dimensions, is sandwiched
between the two Cu substrates. The length of the solder joint
is ensured by placing two equal-thickness aluminum spacers
on either side of the solder;
(4) The joint is maintained in place using a specially designed fixture
made of aluminum plates. The aluminum fixture is used to
prevent any relative movement between the specimen's parts
during the reflow process in the oven when they are heated up
to 30 °C higher than the melting points of the solder materials
(226 °C for SAC-Bi and 218 °C for INNOLOT). The total reflow
time is 5.5 min which includes pre-heating, reflow and cooling
steps. The duration at the melting temperature level is 75 s and
the cooling rate for these solders is determined at 3–4 °C/s ac-
cording to the solder manufacturers’ recommendations.
(5) Finally, before testing, the solder joint samples are ground and
polished again with SiC papers. The different steps of the

Fig. 1. The procedure for fabricating lap shear joint specimens and their dimensions.
406 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416
Table 2.
The shear test matrix.
Strain rate (s  1) 2.0
10  4 2.0
10  3 2.0
10  2
Room (25 °C) X X X
75 °C X X X
125 °C X X X
process, along with the dimensions for the specimens, are
given in Fig. 1.
3. Methodology for shear tests
The shear tests were conducted at three different temperatures
(room temperature, 75 °C and 125 °C). At each temperature, three
different displacement rates were used which corresponds to
three shear strain rates of 2.0
10  4 s  1, 2.0
10  3 s  1 and
2.0
10  2 s  1. A micro-tension tester, with high precision and
resolution for load and displacement, was used to conduct the
shear tests. Details related to the operating principle of a micro-
tension tester can be found in [41,42]. In order to obtain accurate
measurements, a Linear Variable Differential Transformer (LVDT)
and a miniature load cell sensor were used and mounted on the
tester. The sensors were connected to the conditioner devices and
then calibrated before testing. The testing temperature can be
controlled using a heating foil and is monitored by using a ther-
mocouple attached to the sample. The data were collected with a
Data Acquisition (DAQ) device from National Instruments and
treated with the LabVIEW program. The shear joint test matrix and
the experimental setup for shear joints are shown in Table 2 and
Fig. 2., respectively.
The shear strain rates are obtained by dividing the appropriate
displacement rates imposed to the cross-head by the actual solder
joint thickness. In the lap-shear tests, the shear stress and shear
strain of the joint are directly determined from the applied load
and displacement, respectively. Indeed, the average shear stress in
the solder can be taken as the applied axial load divided by solder
joint area in contact with the Cu substrates. The shear strain in the
solder joint was calculated by dividing the actual displacement by
the joint thickness. The average shear stress and shear strain are
thus given by the relations in Eq. (1).
Fig. 2. Micro-tension tester setup.
F ⎛δ ⎞ δ
τ= , γ = tan−1⎜ ⎟ ≈
A ⎝t ⎠ t (1)
where F is the axial load, A is the soldering area, δ is the imposed
displacement and t is the joint thickness.
4. Results and discussion
4.1. Microstructure analysis for some samples
For the microstructural analysis, the solder samples were em-
bedded in epoxy and cut. The surfaces were then polished. Polishing
involves the use of abrasives, suspended in a solution, on a cloth-
covered electrically powered wheel. After each polishing step, the
specimen were carefully washed with water and dried. The speci-
men were ground down to #4000 grit using silicon carbide papers
under ambient temperature water flowing. Next, 3-mm abrasive
diamond particles and dedicated cloth and lubricant were used for
polishing. The final polishing step was applied using colloidal silica
suspension. Cross sectioned surfaces were eventually ready for
high-magnification SEM investigation. In this study, the micro-
structures of the SAC-Bi and INNOLOT joint specimens were in-
vestigated using SU1510 Scanning Electron Microscope Hitachi.
In this study, the composition of the alloys and the stoichio-
metry compounds have been determined by energy dispersive
X-ray spectroscopy (EDX) and EPMA microanalyses, respectively.
These findings were also confirmed in previous works where the
composition of such alloys was established [43].
Firstly, microstructure analyses were done for both solder alloys
as-fabricated. Fig. 3 shows the global views after reflowing of (a) the
SAC-Bi and (b) INNOLOT solder joints; and the IMC phases located
at the upper and lower interfaces with the copper substrates. The
microstructures of both materials consist of large primary β − Sn
grains and intermetallic (IMC) phases. In the case of the SAC-Bi
lead-free solder, the microstructure shows the same features for
β − Sn grains with that of the INNOLOT but differs for the IMCs. Two
types of compounds, Ag3Sn and Cu6Sn5, are found in IMCs of the
SAC-Bi solder, while the INNOLOT solder is concerned with Ag3(Sn,
Sb) and (Cu, Ni)6Sn5 characterized by a finer microstructure due to
the addition of Ni and Sb elements. The IMC (Cu, Ni)6Sn5 is needle-
like in INNOLOT, whereas Cu6Sn5 is globular-like in SAC-Bi.
Moreover, the addition of minor Ni element in the INNOLOT
solder significantly decreases the grain size of the IMC phase. In-
deed, the grain size of (Cu, Ni)6Sn5 particles in the INNOLOT joint is
 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416 407

Fig. 3. The global view of the lap shear joints and the IMC morphology: (a) SAC-Bi (b) INNOLOT.
408 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416

Fig. 4. Cross-sectional SEM images after a shear test at strain rate of 2.0
10  4 s  1 and room temperature for SAC-Bi solder joint.

Fig. 5. Cross-sectional SEM images after a shear test at strain rate of 2.0
10  4 s  1 and room temperature for INNOLOT solder joint.
 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416
Fig. 6. Cross-sectional SEM images after a shear test at strain rate of 2.0
10  4 s  1 and 125 °C for SAC-Bi solder joint.
much smaller than Cu6Sn5 in the SAC-Bi joint (see also Fig. 3). This
is because some of the Cu atoms were replaced by Ni atoms during
the crystallization of Cu6Sn5 due to the similar atom size between
Cu and Ni. Furthermore, Bi (white in color) was precipitated and
appears in the Sn matrix in small and isolated clusters in both
solders as a Sn(Bi) solid solution and dispersion. As for Sb atoms in
the INNOLOT (1.54 wt%), they are in solution into the β − Sn ma-
trix with Ag3(Sn, Sb) phases which not only contribute to suppress
the coarsening of Ag3Sn phase, but also provides solid solution
strenthening.
A type of IMC is formed during the reflow process due to
atomic migration between the Cu substrates and the molten solder
alloy at the interfaces. It is worth noticing that the Cu6Sn5 layer is
formed in SAC-Bi (and (Cu, Ni)6Sn5 in INNOLOT) in the early stages
of the soldering process [40]. Then, the layer grows by consuming,
from the solder the Sn, Cu and Ni atoms leading to the formation
of long dendrites. When the dendrites become too long, they move
away from the IMC interfacial layer and formed some spalled
globular IMC phases that diffuse inside the joint [44].
Secondly, following the shear tests, the fractured micro-
structures have been analyzed. It is well known that the fracture
409
pattern can be classified into three types: ductile fracture inside
the solder, brittle fracture in the solder or at the IMC interface, and
mixed-mode fracture which combines these two types. In this
paper, it is noted that the cracks propagate along the weakest path
which is not similar in the SAC-Bi and INNOLOT solder joints.
Figs. 4 and 5 show the fractography of the SAC-Bi and INNOLOT
alloys after shear testing under the lowest strain rate
(2.0
10  4 s  1) at room temperature (25 °C) with different re-
gions of rupture areas. It can be seen that the Sn phase becomes
elongated for both solder joints and the rupture was initiated in
both cases inside the solder joint before reaching the interface
with the IMC layer, resulting in a mixed-mode fracture (third
type). In addition, some vacancies appear locally near the interface
with the IMC layers. These vacancies may originate from the Kir-
kendall diffusion effect. Indeed, the growth of (Cu, Ni)6Sn5 (IN-
NOLOT) and Cu6Sn5 (SAC-Bi) IMC layers, at the interface with the
solder, strongly consumes the low amount of Cu contained in the
solder which may lead to vacancies formation at the interface on
the solder side, and to local mechanical weakening of the material.
In the vicinity of the rupture area inside the solder joint, the Sn
phases originally globular (before mechanical test) have
410 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416
Fig. 7. Cross-sectional SEM images after a shear test at strain rate of 2.0
10  4 s  1 and 125 °C for INNOLOT solder joint.
undergone an axial growth (long orientated phases) activated by
the mechanical energy applied during the test. However, there are
some differences in the microstructures between the two solder
joints after shearing as represented in the detailed views of the
rupture areas of SAC-Bi and INNOLOT in Figs. 4 and 5, respectively.
In the case of the SAC-Bi, the rupture area can be decomposed into
three zones: (i) at the beginning, the rupture area in the solder
joint appears irregular, suggesting a ductile rupture behavior, (ii)
then the path follows the interface with the thinnest intermetallic
layer, suggesting in this case a fragile transition in the behavior,
(iii) finally, the rupture area ends inside the solder joint with a
more regular rupture area than initially, and so in a more brittle
mode. In the case of the INNOLOT, the rupture area is regular
throughout the propagation, which is an indication of a more
brittle alloy.
Figs. 6 and 7 show the global and cross-sectional SEM images
after shear testing under the lowest strain rate of 2.0
10  4 s  1 at
the highest temperature of 125 °C for SAC-Bi and INNOLOT, re-
spectively. For both solder joints, the rupture occurs faster when
temperature is increased and the Kirkendal voiding effect is more
important in the IMC layer. In the case of SAC-Bi, the irregular
fracture path starts inside the solder joint and is then followed by
a more regular fragile rupture (see the global image in Fig. 6).
Furthermore, it is noted that the fine interdendritic Ag3Sn phases
coalesce to make lager Ag3Sn globular phases. Indeed, the rupture
seems to occur in the area where this transformation occurs. In the
case of the INNOLOT solder joint, there is a fragile rupture at the
IMC interfaces and the type of failure is similar with that of the
test at room temperature under the same strain rate. The fragile
rupture at the IMC interfaces could be due to Kirkendall voiding
near Ag3(Sn, Sb) and (Cu, Ni)6Sn5 particles. However, the Ag3(Sn,
Sb) phases shape transformation is not observed in the rupture
area.
4.2. Shear test results and effect of alloy additions
Fig. 8(a) and (b) represent the shear stress vs. shear strain plots
for SAC-Bi and INNOLOT lap shear solder joint specimens that
were tested at different strain rates and room temperature (25 °C).
Fig. 9(a) and (b) show the plots of the shear stress vs. shear strain
of the two joints obtained for different temperatures ranging from
25 °C to 125 °C and at the lowest strain rate of 2.0
10  4 s  1. It
can be seen that the mechanical properties of both solders are
greatly affected by the alloying elements, strain rates and tem-
peratures. In order to have a more complete view of the effect of
these factors at various testing conditions on the UTS and σy , these
latter quantities are plotted against testing temperature at differ-
ent strain rates in Figs. 10 and 11. As observed, the values of UTS
and σy decrease with the increase of the temperature from room
temperature to 125 °C and increase with the decrease of the shear
strain rate from 2.0
10  4 s  1 to 2.0
10  2 s  1. Also, the alloys
considered here can sustain a large level of deformation before
exhibiting gradual softening until rupture. The UTS are nearly
53.25 MPa and 57.96 MPa under the highest strain rate value of
2.0
10  2 s  1 and at room temperature for SAC-Bi and INNOLOT
solder joints, respectively. In contrast, the lowest shear strength
values of 18.11 MPa for SAC-Bi and 21.15 MPa for INNOLOT were
recorded for the lowest strain rate value of 2.0
10  4 s  1 and at
temperature of 125 °C. The variation tendency of the UTS and σy
can be explained by the microstructural features that were already
discussed above. The addition of a greater quantity of Ni and Sb
clearly enhance the shear strength of the solders as exhibited by
INNOLOT. At as-reflowed condition, the shear strength of INNOLOT
solder joint (with addition of 1.54 wt% Sb and 0.2 wt% Ni), exceeds
by 8.85% that of the original SAC-Bi alloy. In the INNOLOT solder
joint, the formation of finer IMCs, as well as a much smaller grain
size of Ag3(Sn, Sb) and (Cu, Ni)6Sn5 particles, contribute to improve
the mechanical properties. Indeed, according to the investigations
 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416
Fig. 8. Shear stress-strain curves at different strain rates under room temperature
for (a) SAC-Bi solder joint and (b) INNOLOT solder joint.
on this subject in [45], these fine strengthening precipitates can
effectively obstruct the dislocation movement initiated in Sn ma-
trix which leads to the increase of the effective properties of the
alloy. Therefore, the strength of INNOLOT benefits from the par-
ticle hardening caused by Ag3(Sn, Sb) and (Cu, Ni)6Sn5, as well as
some solid solution hardening and refinement by Sb elements.
These are the main evidences to account for the improved strength
of INNOLOT compared to SAC-Bi.
4.3. Identification of the viscoplastic properties of the solder alloys
In literature, numerous material models have been presented
to describe the elastic, elastic-plastic, creep and viscoplastic be-
haviors [34,46–48]. The most popular model for describing the
viscoplastic behavior of solders is the Anand model [49]. Firstly, it
does not require an explicit yield condition nor a loading/un-
loading criterion. It also uses a single scalar internal state variable
and allows an easy identification procedure based on the mono-
tonic or creep tests which can be performed at different strain
rates, applied creep loads and temperatures. Finally, the Anand
model provides rather good estimations based on a unified law for
the inelastic strain in comparison with some decoupled models for
plasticity and creep deformations [50]. Table 3 indicates the ma-
terial parameters of the Anand constitutive law for different lead-
free solders and conventional SnPb alloys. However, to our
411
Fig. 9. Shear stress-strain curves at different testing temperatures under the strain
rate of 2.0
10  4 s  1 for (a) SAC-Bi solder joint and (b) INNOLOT solder joint.
knowledge, no studies exist in literature with regard to the con-
stitutive creep laws of SAC-Bi and INNOLOT new solder alloys. In
this work, the Anand parameters were identified for both alloys to
represent their complex temperature- and strain rate-dependent
behavior.
The obtained data from the shear tests are usually converted
into equivalent tensile stress-strain curves on which the material
parameter identification is performed. Specifically, the tensile
quantities (stress and strain) are estimated based on (Von Mises
criterion):
1
σ= 3τ , ε= γ
3 (2)
where σ , ε are the calculated tensile stress and strain, respectively,
and τ , γ are the shear stress and strain measured during the shear
tests. The details of the Anand model can be found in [49]. The first
differential equation of th eAnand model relates the inelastic
strain rate to the stress:
1
dεin ⎡ ⎛ ⎛ σ ⎞⎞⎤ m
= A⎢ sinh⎜ ξ ⎜ ⎟⎟⎥ exp( −Q /RT )
dt ⎣ ⎝ ⎝ s ⎠⎠⎦ (3)
The model consists of nine material parameters. The function
lsqcurvefit in the Matlab commercial tool was used due to its
412 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416

Fig. 10. Dependence of UTS on strain rate at different testing temperatures for
(a) SAC-Bi solder joint and (b) INNOLOT solder joint. Fig. 11. Dependence of yield stress on strain rate at different testing temperatures
for (a) SAC-Bi solder joint and (b) INNOLOT solder joint.

ability to solve non-linear data fitting problems in the least

squares sense. The procedure of the determination of Anand’s Using the fitting procedure described above, the nine Anand
material parameters is as follows: model material parameters were estimated and listed in Table 4.
The quality of fitting is verified against experimental data for dif-
^ ferent temperatures and strain rates as shown in Figs. 12 and 13.
(1) In the first stage, five parameters (A, Q , s , n and m ) are esti-
R ξ
mated by non-linear least squares fitting of Eq. (4) that is The fittings show that the experimental stress-strain data matched
derived from Eq. (3) and gives the saturation stress σ * as well with the simulated results based on the Anand model. It
function of the inelastic strain rate ε̇p and temperature T. should also be noted that the material constants estimated for the
two alloys are in the same order of magnitude as values found in
s^ ⎛ εṗ Q / RT ⎞
n ⎡ ⎛ ε̇ ⎞m⎤ the literature for other SAC alloys [51].
p
σ* = ⎜ e ⎟ sinh−1⎢ ⎜ eQ / RT ⎟ ⎥
ξ⎝ A ⎠ ⎢⎣ ⎝ A ⎠ ⎥⎦ (4)
4.4. Simulations of thermal cycling on an electronic assembly
s^
For this stage, it must be emphasized that the ratio is used as
ξ
a single unknown variable. Based on the viscoplastic Anand constitutive model identified
(2) In the second stage, the remaining parameters (h0, c and a ) in this study, Finite Element Method (FEM) analysis is used to
are determined by non-linear least squares fiting of Eq. (5) evaluate thermal-mechanical behavior of the SAC-Bi and INNOLOT
giving the stress as function of the inelastic strain at several solder joints that are used in Insulated Gate Bipolar Transistor
strain rates and temperatures: modules (IGBT).

1/ (1 − a)
⎡
(
σ = σ * − ⎢⎣ σ * − cs0 )
(1 − a )
( −a
+ (a − 1) (ch0)(σ *) )ε ⎤⎥⎦
p ,
4.4.1. Module geometrical model
Fig. 14 shows a schematic of the basic IGBT structure and Ta-
1 ⎡⎛ ε˙ Q ⎞m⎤ ble 5 indicates the dimensions (length, width and thickness) of all
p
c= sinh−1⎢⎜ e RT ⎟ ⎥ components in the module. In this type of module, there are two
ξ ⎢⎣⎝ A ⎠ ⎥⎦ (5) solder layers, one for the die attachment (upper layer) and one for
 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416 413

Table 3.
Anand material parameters for several solder alloys.

Solder alloys A (s  1) Q/R (K) ξ m s^ (MPa) n h0 (MPa) a s0 (MPa)

Sn3.8Ag0.7Cu 24,300 8710 5.8 0.183 65.3 0.019 3541.2 1.9 39.5
Sn3.8Ag0.7Cu0.03Ce 21,200 8026 5 0.130 57.6 0.0175 4352.6 2.3 28.5
Sn3.5Ag 177,016 85,459 7 0.207 52.4 0.0177 27,782 1.6 0.0673T þ 28.6
Sn3.8Ag0.7Cu 15.773 9883 1.0673 0.3686 3.1505 0.0352 1076.9 1.6832 3.2992
Sn1.0Ag0.5Cu 3.773 8076 0.9951 0.4454 3.5833 0.0120 4507.5 2.1669 2.3479
Sn3.0Ag0.5Cu 717.260 6067 2 0.130 29.0 0.0436 14,560 2.22 2.45
Sn3.5Ag 344.716 6538 3 0.143 26.0 0.0447 23,241 1.46 0.65
Sn0.7Cu 764.166 5837 2 0.123 26.4 0.0430 11,656 2.33 4.43
Sn3.8Ag0.7Cu 107.65 7619 59.36 4.03 86.28 0.0046 9002 1.30 22.64
Sn4.0Ag0.5Cu 325 10,561 10 0.32 42.1 0.02 800,000 2.57 20
Sn3.8Ag0.7Cu 2.23 8900 6 0.182 73.81 0.018 3321.15 1.82 39.09
Sn37Pb 6220 6525 3.33 0.27 36.86 0.022 60,599 1.7811 3.1522
Sn8.5Sb 2.23E8 13816.8 13.85 0.417 76.0 0.01 291,215 2.34 48.15
Sn92.5Pb2.5Ag 105,200 11,010 7 0.241 41.63 0.002 1432 1.3 33.07
Sn3.8Ag0.7Cu0.8Zn 23,500 8500 5.6 0.163 65.9 0.0186 3642.5 2.1 34.1
Sn3.0Ag0.5Cu 17.994 9970 0.35 0.153 2.536 0.028 1525.98 1.69 2.15

Table 4.
The Anand model parameters determined for SAC-Bi and INNOLOT from stress-strain data.

Constant Number Anand Constant Units Description SAC-Bi INNOLOT

1 s0 MPa Initial value of deformation resistance 20.5280 52.7256

2 Q/R K Activation energy/boltzmann's constant 8850.7 9059.6
3 A Section  1 Pre-exponential factor 15.25 15.25
4 ξ Dimensionless Stress multiplier 1.1395 1.1026
5 m Dimensionless Strain rate sensitivity of stress 0.1373 0.0245
6 h0 MPa Hardening/softening constant 7379.5 9561.6
7 s^ MPa Coefficient for saturation value of deformation resistance 12.1797 19.5959
8 n Dimensionless Strain rate sensitivity of the saturation value 0.0367 0.0611
9 a Dimensionless Strain rate sensitivity of the hardening/softening 1.8055 1.5820

the substrate to base plate attachment (bottom layer).
The Abaqus commercial software was used to create the FEM
model of the IGBT module. Fig. 15 (a) and (b) show the geometrical
model and the finite element meshing. There are 76,592 nodes and
59,100 elements for the complete meshing of the assembly.
The behaviors of both solder layers in the module (taken con-
secutively as SAC-Bi and INNOLOT for comparison) are taken as
viscoplastic and following the same Anand law identified pre-
viously. Concerning the properties of the materials used for the
other components (silicon chip, copper, aluminum and epoxy),
they are treated as linear elastic materials and taken as dependent
on temperature. The treatment of creep in the finite element cal-
culations is done with the help of a Fortran subroutine that we
have implemented in Abaqus.
4.4.2. Profile of the thermal loading
It is known that during service, the power module is subjected
to both active (power cycling) and passive cycles (variation of
ambient temperature). However, in this study the focus is put on
the effects of passive thermal cycles which are characterized by far
higher temperature variations than those resulting from current
circulation. In terms of deformation, strains and stresses which
appear in the solder material under this type of loading (thermal
shocks) are expected to be elevated and thus need to be correctly
evaluated for reliability assessment. The temperature cycles ap-
plied in the simulation are in the range of 10 °C to 80 °C which is
similar to the operating temperature in devices as shown in Fig. 16.
The whole thermal cycle includes ramp-up, dwell and ramp-down.
The dwell period is 15 min at the peak of each cycle, while the
heating and cooling rates are 2.33 °C/min and 1.78 °C/min, re-
spectively. This thermal cycle profile is taken to be representative
of the constraints that the commercially available IGBT modules
have to experience in their lifetime.
4.4.3. Numerical results
Fig. 17 shows the FEM results for the accumulated inelastic
energy in the two solder layers based on the Anand model for the
SAC-Bi and INNOLOT alloys, respectively. The most critical regions
are located at the corners of the solder layers which are near the
interfaces with the DBC substrate and the base plate. The max-
imum Von Mises stress of the INNOLOT solder joint is higher than
that of the SAC-Bi solder joint, 52.46 MPA and 47.71 MPa, respec-
tively. Fig. 18 represents the accumulated plastic strains at the
critical locations. It is observed that the accumulated plastic strain
in the INNOLOT solder joint is lower than that of the SAC-Bi solder
joint, which shows that the INNOLOT alloy, that is stiffer, allows, in
return, less energy dissipation during its solicitation. This suggests
that INNOLOT could behave more efficiently under fatigue if the
energy-based model of Morrow or the plastic strain-based model
of Coffin-Manson were considered to estimate lifetime of the alloy.
These models relate indeed the material lifetime to the plastic
strain amplitude or the dissipated energy, following (in the case of
the Morrow law) the relationship ΔW ⋅N m f = C where ΔW is the
inelastic strain energy density in the stabilized cycle, Nf is the
number of cycles to failure, and m and C represent material
parameters to be identified. Fatigue characterization of the mate-
rials was beyond the goals of the present work but these pre-
liminary FE simulations are the first steps for future investigations
on the alloys fatigue behaviors based on simulations. Such a study
would require cyclic testing of specimens for parameter identifi-
cation useful for the lifetime prediction models.
5. Conclusions
In this paper, shear tests were conducted on joint specimens
based on two new lead-free solder alloys, SAC-Bi and INNOLOT, to
414 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416

Fig. 13. Relations between inelastic strain and stress: comparison between ex-
perimental results and Anand model fits at three strain rates for the temperature
25 °C.

Fig. 12. Plots of the saturation stress versus steady-state strain rate from shear
tests: experimental results and Anand model predictions.

investigate the effect of Ni and Sb additions and that of the testing

conditions (strain rate and temperature) on the mechanical Fig. 14. Schematic of basic IGBT module.
properties and microstructure. The results are summarized as
follows:
Table 5.
(1) The mechanical properties of shear tests are highly dependent Dimensions of the components in the IBGT module.
on atoms addition and testing conditions. The shear strength
of the solder joints will decrease with an increase in tem- Layer Length Width Thickness (mm)
(mm) (mm)
perature and increase with higher strain rate.
(2) The Ni, Bi and Sb additions lead to creation of particular in- Silicon chip 5.383 4.425 0.228
termetallic compounds, Ag3Sn vs Ag3(Sn, Sb), and Cu6Sn5 Top solder (SAC-Bi and 5.383 4.425 0.068
Cu6Sn5 vs (Cu, Ni)6Sn5 for SAC-Bi and INNOLOT, respectively. It INNOLOT)
DBC Substrate-Cu 7.178 8.3 0.300
also improves the shear strength and the Sb-containing solder
DBC Substrate-Alumina 7.178 8.3 0.690
joints (INNOLOT) have higher UTS and σy than Sb-free solder DBC Substrate-Cu 7.178 8.3 0.300
joints (SAC-Bi) due to the solid solution hardening and particle Bottom solder (SAC-Bi and 7.178 8.3 0.123
hardening effect of Sb. INNOLOT)
(3) The material parameters of the viscoplastic constitutive law of Baseplate-aluminum 20 20 1.600
Baseplate-epoxy 20 20 0.078
Anand were identified based on a non-linear least square fit- Baseplate-Cu 7.5 8.4 0.087
ting method of the testing data. The findings in Anand model
are in good agreement with the experimental data and pre-
vious studies for other solder alloys. (5) The as-reflowed and fractured microstructures of the solder
(4) The obtained material parameters of the Anand constitutive joints were investigated at different conditions to understand
model were utilized in a FEM analysis to evaluate the stress- more about the effect of the testing conditions and atoms
strain response of an Insulated Gate Bipolar Transistor under additions on the associated changes of microstructure of the
thermal cycling. solder joints.
 Q.B. Tao et al. / Materials Science & Engineering A 669 (2016) 403–416 415

Fig. 15. Geometrical model of the electronic assembly (a) and its meshing (b).

As perspectives for this study, fatigue characterization of the

alloys must be carried out by applying cyclic loading to the spe-
cimens under several conditions. These tests are necessary to es-
timate reliability of the new alloys subjected to different thermal
cycling as is the case when used as solder joints in power modules.
This will also allow identification of the parameters of some fati-
gue laws required for simulation.

Acknowledgments

The authors would like to thank Dr K.L. Tan and Dr J.M. Morelle
from VALEO company, France for providing us with the solder
materials. This research was supported by the French National
Research Agency ANR and VALEO (Grant no. ANR-12-CHIN-0004).
The authors are also grateful to F. Mourgues for machining the
mechanical components of the fixture holding the substrates with
Fig. 16. Thermal cycling profile.
the solder during reflow.

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