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High Temperature Creep Response of Lead Free Solders

Conference Paper · May 2016

DOI: 10.1109/ITHERM.2016.7517686

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 High Temperature Creep Response of Lead Free Solders
Abdullah Fahim, Sudan Ahmed, Md Mahmudur R. Chowdhury, Jeffrey C. Suhling, Pradeep Lall
Department of Mechanical Engineering, and
Center for Advanced Vehicle and Extreme Environment Electronics (CAVE3)
Auburn University
Auburn, AL 36849
Phone: +1-334-844-3332
FAX: +1-334-844-3124
E-Mail: jsuhling@auburn.edu

ABSTRACT 150-200 oC (TH ≈ 0.85-0.95). Thus, significant creep will

Lead free solder materials are susceptible to significant
creep deformations in harsh high temperature environments
including automotive, avionics, military, and oil exploration
applications. In addition, dramatic degradations will occur in
the creep responses of lead free solder alloys when they are
exposed to long term isothermal aging during product
applications at high temperatures. Such degradations in the
creep compliance of the solder material are universally
detrimental to reliability of solder joints in electronic
assemblies.
In this work, we have characterized the high temperature
creep behavior of SAC405 (95.5Sn4.0Ag0.5Cu) lead free
solder, which is the most creep resistant of the standard
SACN05 alloys. In addition, we have studied the creep
behaviors of two doped SAC solders, SAC_Q and Innolot,
which have been previously shown to out-perform SAC405 in
simple mechanical stress-strain tests at room temperature.
Tensile specimens were formed in rectangular cross-section
glass tubes using a vacuum suction process, and a water
quenched (WQ) solidification profile was utilized to yield fine
microstructures and the upper limits of the mechanical
properties for each alloy. The samples were then aged for 10
days at room temperature to stabilize their microstructures.
After aging, creep testing was performed at two different
stress levels (10, 15 MPa) and several different extreme/high
testing temperatures (T = 100, 125, 150, 175, and 200 oC).
For each set of conditions, the creep performances of the three
alloys were compared. The results showed that the doped
SAC alloys were more resistant to creep at high temperatures.
The creep rates of SAC_Q are roughly 50% of those for
SAC405, while the creep rates of Innolot are roughly 33% of
those for SAC405. It is likely that the dopants can
significantly block the movement of dislocations and thus
increase the creep resistance of these solders.
KEY WORDS: Lead Free Solder, Creep, Aging, Strain Rate
INTRODUCTION
Creep becomes a dominant deformation mode in a solder
material when it’s homologous temperature, TH = T/TMelt >
0.5. For Sn-Ag-Cu (SAC) lead free solders, this condition
occurs at relatively low temperatures (e.g. room temperature,
T = 25 oC, TH ≈ 0.6). Lead free electronics are often exposed
to more severe high temperature environments including
automotive, avionics, military, and oil exploration
applications, where service temperatures can approach T =
easily occur in such harsh environments. In addition,
prolonged exposures at such high temperatures can lead to
excessive aging induced changes to their microstructure and
reductions in their mechanical properties and creep resistance.
The literature on lead free solder materials has shown that
aging is universally detrimental to their constitutive and
failure behaviors [1]. In particular, large degradations have
been observed in ball shear strength [2], elastic modulus [3],
drop reliability [4], fracture behavior [5], microstructure [6],
creep behavior [7-11], thermal cycling reliability [12-16],
Anand model parameters [15-16], nanoindentation joint
modulus and hardness [17-19], high strain rate mechanical
properties [20], uniaxial cyclic stress-strain curves and fatigue
life [21-22], and shear cyclic stress-strain curves and fatigue
life [23-24].
Adding dopants such as Bi, Ni, In, Mg, Mn, Zn, La, Ce,
Co, and Ti to lead free SAC alloys can improve the
wettability, melting temperature, shock/drop reliability, creep
properties, and microstructure [11]. For example, adding
Bismuth (Bi) helps to reduce solidification temperature,
increases strength by means of precipitation hardening, and
also helps to reduce IMC (Intermetallic Compound) layer
thicknesses in lead free solder materials [25]. The Effect of
Bi on the mechanical properties of a SAC (Sn3.5Ag0.9Cu)
alloy was investigated by Matahir and coworkers [26]. They
reported that the shear strength increased with increasing Bi
addition up to 2% (wt). Beyond that point, the shear strength
decreased with increasing Bi%. The improved shear strength
was attributed to the role of Bi on the morphology of the
microstructure and distribution of dominant IMC (Ag3Sn).
Reduction of strength at higher Bi content was due to the
evolution of Bi rich phase and fragmentation of the IMC.
Pandher, et al. [27] also reported that addition of up to 2% Bi
in SAC alloys improved wetting and alloy spreading.
Cai, et al. [11, 28] demonstrated that addition of 0.1% Bi
in SAC0307 solder dramatically reduces aging effects such as
material property degradations by a solid solution
strengthening mechanism. Witkin [29] compared mechanical
properties of SAC305 with two different Bi-doped alloys, and
also concluded that the addition Bi can significantly reduce
aging effects. He also showed that Bi is present in the
microstructure as a separate phase or goes into solid solution
with Sn, and does not form any intermetallic compounds with
Sn, Cu or Ag. Reduction of IMC layer thickness after Bi
addition has also been reported [30-31]

978-1-4673-8121-5/$31.00 ©2016 IEEE 1218 15th IEEE ITHERM Conference

 Dopants are also added to alloys in very small amounts (WQ) solidification profile has been used to solidify the
(microalloy additions). Zhao, et al. [32] found that addition of solder test specimens, which led to fine microstructures and
0.02% Ni to SAC105 increased the formation of NiCuSn IMC the upper limits of the mechanical properties and creep
and reduced the localized grain size at solder/NiAu pad resistance for each alloy. After WQ solidification, all of the
interfaces. In addition, the effects of using various low level samples were aged at room temperature for 10 days before
doping elements (i.e. Co, Fe, In, Ni, Zn, and Cu) in SAC305 testing to stabilize their microstructures. For each solder
BGA solder joints on Cu pads were studied by Sousa, et al. material, creep experiments were performed at 5 different
[33]. They concluded that addition of low levels of Zn had a extreme/high testing temperatures (T = 100, 125, 150, 175,
significant beneficial effect on the interfacial IMC. Lee and and 200 oC), and two stress levels (10, 15 MPa). Five
coworkers [34] found that micro-alloying SAC alloys with Ni specimens were tested for each combination of solder alloy,
and Bi improved thermal fatigue life and drop impact temperature, and stress level. Using the measured creep strain
resistance. Finally, Yeung, et al. [35] worked with a SAC-Bi vs. time data, the secondary creep rates were obtained for both
alloy (SAC_Q), and found enhanced solder joint reliability the standard and doped SAC alloys.
during thermal cycling without affecting reliability in board
level drop tests. Table 1 - Creep Experiment Test Matrix
A six element Sn-Ag-Cu-Bi-Ni-Sb lead free solder alloy
referred to as InnolotTM has been introduced by several solder SAC 405 SAC_Q Innolot
vendors for enhanced high temperature reliability. Dudek, et Temperature σ (MPa) σ (MPa) σ (MPa)
al. [36] investigated the creep responses of Innolot and several T (oC)
other SAC alloys by solder joint shear testing. Their findings 10 15 10 15 10 15
showed that the Innolot alloy had the lowest creep strain rates 100 √ √ √ √ √ √
at both T = 20 oC and T = 150 oC. Miric [37] reported that 125 √ √ √ √ √ √
ceramic chip capacitors assembled with Innolot solder had 150 √ √ √ √ √ √
better thermal cycling reliability than analogous components 175 √ √ √ √ √ √
assembled with several other lead free solders. Tao, et al. [38]
200 √ √ √ √ √ √
tested Innolot lap shear specimens over a temperature range
from 25-125 oC and proposed a creep model to fit their data.
Ahmed, et al. [39] measured stress-strain curves for three The chemical compositions of the doped SAC alloys were
doped SAC alloys including Innolot, SAC_R (EcolloyTM), and determined in our previous study [39] using Energy
SAC_Q (CyclomaxTM). Using the results at 5 different Dispersive X-Ray Spectroscopy (EDX), and are listed in
temperatures and 3 different strain rates, the 9 Anand model Table 2 along with the composition of the traditional SAC405
constitutive parameters were found for each alloy. In alloy. SAC_Q is formulated with Sn, Ag, Cu, and Bi
addition, two of the doped SAC solders (SAC_Q and Innolot) (SAC+Bi), while Innolot includes an engineered combination
were found to out-perform SAC405 in simple mechanical of six elements (Sn-Ag-Cu-Bi-Ni-Sb). The silver contents of
stress-strain tests at room temperature. SAC_Q and Innolot are similar to that of SAC405, at 3.41%
In this work, we have characterized the high temperature and 3.80% respectively.
creep behavior of SAC405 (95.5Sn4.0Ag0.5Cu) lead free
solder, which is the most creep resistant of the standard Table 2 - Chemical Compositions of the Solder Alloys
SACN05 alloys. In addition, we have studied the creep
behaviors of two doped SAC solders (SAC_Q and Innolot), Alloy Sn Ag Cu Bi Ni Sb
based on their potential as shown in the limited previous SAC 405 95.50 4.00 0.50 0.00 0.00 0.00
studies discussed above. Tensile specimens were formed in SAC_Q 92.77 3.41 0.52 3.30 0.00 0.00
rectangular cross-section glass tubes using a vacuum suction Innolot 90.95 3.80 0.70 3.00 0.15 1.40
process, and a water quenched (WQ) solidification profile was
utilized to yield fine microstructures and the upper limits of Uniaxial Test Sample Preparation
the mechanical properties for each alloy. The samples were Bulk solder samples were cut into small pieces and were
then aged for 10 days at room temperature to stabilize their melted into a quartz crucible by induction heating. Molten
microstructures. After aging, creep testing was performed at solder was then drawn into glass tubes with rectangular cross-
two different stress levels (10, 15 MPa) and several different sections by a vacuum suction method [7-11]. The glass tube
extreme/high testing temperatures (T = 100, 125, 150, 175, solder samples were next cooled by water quenching (WQ) to
and 200 oC). For each set of conditions, the creep solidify the solder in the tubes and form the uniaxial tensile
performances of the three alloys were compared and ranked. specimens. Solidified solder test samples were extracted by
breaking the glass tubes. The typical dimensions of the final
EXPERIMENTAL PROCEDURE test samples were 80 x 3 x 0.5 mm, and the gage length during
the uniaxial testing was 60 mm. After solidification, the
Test Matrix samples were aged at room temperature for 10 days before
The test matrix of creep experiments for the standard and testing to stabilize the microstructure. After aging, the test
doped lead free SAC solder alloys (SAC405, SAC_Q, and samples were kept in low temperature freezer to eliminate or
Innolot) is shown in Table 1. In this study, a water quenched minimize further aging induced changes before creep testing
Mechanical Testing System
The MT-200 tension/torsion thermo-mechanical test
system from Wisdom Technology, Inc., shown in Figure 1
was used to perform the creep testing in this work. The
system provides an axial displacement resolution of 0.1
micron, and universal 6-axis load cell was utilized to
simultaneously monitor three forces and three moments
during sample mounting and testing. Use of the pictured
heating chamber allowed samples to be tested up to +200 °C.
Figure 1- Mechanical Test System with Solder Sample
Typical Creep Test Data
Figure 2 illustrates a typical creep curve (strain vs. time
response for a constant applied stress) for a SAC solder
material. Under constant uniaxial stress, the creep response
begins with a quick transition to the initial “elastic” strain
level. This jump is followed by regions of primary,
secondary, and tertiary creep. The secondary creep region
often contains a nearly constant slope over a very long
duration. This slope value is referred to as the “steady state”
secondary creep strain rate. Practicing engineers often use
this creep rate as one of the key material parameters for solder
in finite element simulations used to predict solder joint
reliability.
Figure 2 - Typical SAC Solder Creep Curve
Creep Data Processing
The experimental creep data from each test were fit with
an empirical model to obtain a numerical representation of the
data and to extract the secondary creep rate. The raw strain
versus time data in the primary and secondary creep regions
were found to be well fitted by the creep response of the four
parameter Burger’s (spring-dashpot) model:
ε  C 0  C1 t  C 2 (1  e  C 3 t ) (1)
where C0, C1, C2 and C3 are fitting constants. Note that
constant C1 gives the slope of curve in the secondary creep
zone for large times. Figure 3 shows a regression fit of the
model in eq. (1) to a typical set of creep strain vs. time data.
Figure 3 - Empirical Model Fit to Experimental Creep Data
CREEP TEST RESULTS
Figures 4a, 4b, and 4c illustrate typical recorded creep
curves at the fixed stress level of 10 MPa for the SAC405,
SAC_Q, and Innolot solder materials, respectively.
Analogous results for the stress level of 15 MPa are presented
in Figures 5a, 5b, and 5c. The five colored curves in each plot
are for the five different testing temperatures (T = 100, 125,
150, 175, and 200 oC). At the higher stress level, dislocation
movement due to creep became more significant, which
resulted in higher creep rates for all of the alloys. At higher
temperatures, the movement of dislocations is enhanced, and
more creep results.
By visually comparing the analogous curves for the 3
alloys (same stress level and temperature), it can be seen that
SAC405 has the highest creep rates (slopes) for all of the
considered temperatures and stress levels. In addition, the
Innolot alloy has the lowest creep rates (slopes) for all of the
considered temperatures and stress levels. The average
extracted secondary creep rates are presented in Table 3, and
plotted in Figure 6. The creep rates of SAC_Q are roughly
50% of those for SAC405, while the creep rates of Innolot are
roughly 33% of those for SAC405.
 (a) SAC 405 (a) SAC 405

(b) SAC_Q (b) SAC_Q

(c) Innolot (c) Innolot

Figure 4 - Creep Curves for  = 10 MPa Figure 5 - Creep Curves for  = 15 MPa
 Table 3 - Average Secondary Creep Strain Rates Innolot alloy can replace the Cu atoms in the Cu6Sn5 phases
and generate new (Cu, Ni)6Sn5 IMC phases that help block
Secondary Strain Rate dislocation movements. Also the presence of Sb in Innolot
T σ (x 10-8 sec-1) could suppress the coarsening of the β-Sn phases and refine
o
( C) (MPa) the Ag3Sn precipitates, and thus improve the mechanical and
SAC 405 SAC_Q Innolot thermal properties of the Sn-based solders.
10 19.7 8.4 2.4
100
15 57.7 33.1 16.1 SUMMARY AND CONCLUSIONS
10 45.4 20.3 7.4 In this work, we have characterized the high temperature
125
15 154.0 79.6 40.9 creep behavior of SAC405 (95.5Sn4.0Ag0.5Cu) lead free
10 87.7 46.3 18.7 solder, which is the most creep resistant of the standard
150
15 364.0 190.0 102.0 SACN05 alloys. In addition, we have studied the creep
10 164.0 82.1 54.9 behaviors of two doped SAC solders, SAC_Q and Innolot,
175
15 697.0 394.0 288.0 which have been previously shown to out-perform SAC405 in
10 234.0 156.0 81.0 simple mechanical stress-strain tests at room temperature.
200
15 1190.0 883.0 611.0
Tensile specimens were formed in rectangular cross-section
glass tubes using a vacuum suction process, and a water
quenched (WQ) solidification profile was utilized to yield fine
microstructures and the upper limits of the mechanical
properties for each alloy. The samples were then aged for 10
days at room temperature to stabilize their microstructures.
After aging, creep testing was performed at two different
stress levels (10, 15 MPa) and several different extreme/high
testing temperatures (T = 100, 125, 150, 175, and 200 oC).
For each set of conditions, the creep performances of the three
alloys were compared. The results showed that the doped
SAC alloys were more resistant to creep at high temperatures.
The creep rates of SAC_Q are roughly 50% of those for
SAC405, while the creep rates of Innolot are roughly 33% of
those for SAC405. It is likely that the dopants can
significantly block the movement of dislocations and thus
increase the creep resistance of these solders.
(a) = 10 MPa
ACKNOWLEDGMENTS
This work was supported by the NSF Center for Advanced
Vehicle and Extreme Environment Electronics (CAVE3).

(b)  = 15 MPa
Figure 6 - Variation of Creep Strain Rate with Temperature
Further study is necessary to fully understand the exact
microstructural mechanisms responsible for the improved
creep resistances of the doped alloys. One likely reason is
that the presence of the additional alloying elements can block
more dislocation movements relative to SAC405. In addition,
dopants such as Bi and Sb can go into solution with tin,
providing solid solution strengthening. Ni present in the
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