metals

Article
Creep Properties Assessment by Shear Punch Creep
Test and IMC Morphology of Aged Pb-Free Solder
Joint/UBM
Sophal Hai and Hyo-Sun Yu *
Division of Mechanical System Engineering, Chonbuk National University, Automotive Technology Research
Center, 567 Baekje-daero, Deokjin-gu, Jeonju-si, Jeollabuk-do 54896, Korea; khaisophal@naver.com
* Correspondence: hyosun4029@naver.com; Tel.: +82-63-270-2346




Received: 8 January 2019; Accepted: 29 January 2019; Published: 11 February 2019


Abstract: In this paper, we investigated the intermetallic compound (IMC) morphology of aged
(0, 200, 600 h) conventional Sn-37Pb and Pb-free Sn-4Ag-0.5Cu solder joints/(Ni-P/Au) UBM; the
creep properties of the solder joints were evaluated using a shear punch creep test (SPCT) method.
The creep displacement-time curves of the solder joints exhibited different behaviors depending
on stress application and aging treatment conditions. Empirical formulas such as the Power-law
and Monkman-Grant relationship have been used to analyze the SPCT data. Furthermore, the IMC
behavior of solder joints was investigated using energy-dispersive X-ray spectroscopy (EDS) and a
scanning electron microscope (SEM). The result showed that with an increase of the aging time, the
stress exponents (n) of solder joints were decreased, but the IMC thickness and size were increased.
In most of the experimental conditions, the creep properties of Pb-free solder joints were superior to
the conventional Sn-37Pb solder joints.

Keywords: Pb-free solder joint; aging treatment; IMC; UBM; shear punch creep test (SPCT); creep

1. Introduction
Conventional Sn-Pb solder joints are commonly used as the most outstanding solder joint for
the electronic packaging industry. Over the past decades, they have been used as the most effective
bonding material of electronic devices due to their excellent mechanical properties such as a low
melting point, wettability and fatigue resistance, and low cost [1,2]. However, conventional Sn-Pb
solder alloys are treated as general waste and therefore have bad effects on the environment, such as
air and water pollution; they especially have a bad effect on human health [3].
As a result, the European Union (EU) has enacted environmental regulations, which include the
restriction of hazardous substances (RoHS), as well as the waste electrical and electronic equipment
(WEEE) legislation, to forbid the use of lead (Pb) in electrical and electronic products. For that reason,
research on Pb-free solder has received much widespread attention [4,5]; in particular, Sn-Ag-Cu solder
alloys are currently known as being the most promising Pb-free solder joints [6]. Sun et al. [7] suggested
that in the reflow processing, the eutectic Sn-Pb solder joints can be replaced with a eutectic Sn-Ag-Cu
solder joint. In addition, for the wave soldering process, the eutectic Sn-Pb solder joint can possibly
be replaced with the eutectic Sn-Cu alloy as well. In the electronic packaging, Ni-P/Au multilayers
have been considered as a promising UBM with a micro-solder bump for flip chip technology due
to their functions. This is because they have provided a good solderable surface and also have a
function for protecting the underlying copper (Cu) from reacting with the solder, at a low-cost [8]. The
IMC behavior is considered a crucial factor for predicting the mechanical properties of solder joints.
After 200 ◦ C HTS aging, the phase microstructure, thickness, and fracture morphology of IMC on the

Metals 2019, 9, 209; doi:10.3390/met9020209 www.mdpi.com/journal/metals

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morphology of IMC on the interface of SAC solders/UBM have an influence on the pull strength of
the joint [9]. On the other hand, the shear punch creep test method has been investigated by many
interface of SAC solders/UBM have an influence on the pull strength of the joint [9]. On the other
researchers for over twenty years, and it has been applied to evaluate the ductile and brittle materials.
hand, the shear punch creep test method has been investigated by many researchers for over twenty
As a result, this method is considered as an acceptable tool for determining material creep properties
years, and it has been applied to evaluate the ductile and brittle materials. As a result, this method is
[10]. However, there have been few reports about applying this creep test method using the SPCT for
considered as an acceptable tool for determining material creep properties [10]. However, there have
solder joints.
been few reports about applying this creep test method using the SPCT for solder joints.
The main purpose of this study is to assess and investigate the creep mechanical properties of
The main purpose of this study is to assess and investigate the creep mechanical properties
aged Pb-free Sn-4Ag-0.5Cu solder joints/(Ni-P/Au) UBM using the SPCT method at 30 °C. The
of aged Pb-free Sn-4Ag-0.5Cu solder joints/(Ni-P/Au) UBM using the SPCT method at 30 ◦ C. The
isothermal aging was conducted at 150 °C during 0, 200, 600 h. Furthermore, the IMC behavior of
isothermal aging was conducted at 150 ◦ C during 0, 200, 600 h. Furthermore, the IMC behavior of
solder joints was observed using SEM and EDS. The mechanical properties of Pb-free Sn-4Ag-0.5Cu
solder joints was observed using SEM and EDS. The mechanical properties of Pb-free Sn-4Ag-0.5Cu
solder joints were compared with the conventional Sn-37Pb solder.
solder joints were compared with the conventional Sn-37Pb solder.
2.
2. Experimental
Experimental Section
Section and
and Preparation
Preparation of
of Test
Test Specimens
Specimens

2.1.
2.1. Materials
Materials and
and Preparation
Preparation of
of Test
Test Specimens
Specimens
In
In this
this research,
research, the
the conventional
conventional Sn-37Pb
Sn-37Pb solder
solder joints
joints and
and Pb-free
Pb-free Sn-4Ag-0.5Cu
Sn-4Ag-0.5Cu solder
solder joints
joints
were
were used
used to
to evaluate
evaluate the
the creep
creep properties
properties of of the
the solder
solder joint.
joint. Figure
Figure 11 shows
shows the
the fabrication
fabrication process
process
of
of the
the specimen
specimen for for the
the SPCT
SPCT method.
method. (Step.
(Step. 1)1) The
The CuCu substrates
substrates were
were machined
machined and and polished
polished by by
sandpaper
sandpaper from # 800 to # 2000 grit, to obtain a 10 × 10 × 0.8 mm size and a center hole ofØ3.2
from # 800 to # 2000 grit, to obtain a 10 × 10 × 0.8 mm size and a center hole of Ø3.2mm.mm.
(Step.
(Step. 2)2)Multi-layers
Multi-layersofofNi-P/Au
Ni-P/Au UBM,
UBM, about
about5 and
5 and0.1 0.1
μm,µm,respectively,
respectively, were deposited
were depositedon the
on Cuthe
substrates. (Step. 3) The solder balls were reflowed into the Cu substrate at
Cu substrates. (Step. 3) The solder balls were reflowed into the Cu substrate at reflow temperature reflow temperature (Sn-
37Pb: 200 °C,
(Sn-37Pb: 200Sn-4Ag-0.5Cu:
◦ C, Sn-4Ag-0.5Cu: 240 °C)240for 30for
◦ C) s and
30 were
s andcooled at room
were cooled at temperature for 10 min.
room temperature for 10(Step.
min.
4) The 4)
(Step. surfaces of specimens
The surfaces were polished
of specimens to obtain
were polished a final asize
to obtain (10size
final × 10(10
× 0.5
× 10mm). (Step.
× 0.5 mm). 5) (Step.
Finally, 5)
SP specimens were treated to isothermal aging (AJ-SB4/9908) at 150 °C for
Finally, SP specimens were treated to isothermal aging (AJ-SB4/9908) at 150 C for 0, 200, and 600 h. ◦0, 200, and 600 h. The
chemical composition
The chemical of theof
composition solder joints is
the solder shown
joints in Table
is shown in1.Table
The experiment conditions
1. The experiment and melting
conditions and
point temperature of the solder joints is summarized in
melting point temperature of the solder joints is summarized in Table 2. Table 2.

Figure 1.
Figure Schematic view
1. Schematic view for
for SPCT
SPCT specimen
specimen machining.
machining.

Table 1. The chemical composition of solder joints.

Table 1. The chemical composition of solder joints.
Chemical Composition (wt. %)
Solder Joint
Chemical Composition (wt. %)
Solder Joint Sn Pb Sb Cu Bi Zn Fe Al As Cd Ag Ni
Sn-37Pb 62–64Sn Bal-Pb 0.10
Sb Cu
0.03 Bi
0.03 Zn
0.002 Fe
0.02 Al
0.002 As
0.03 Cd
0.002 Ag
0.002 Ni
0.01
Sn-4Ag-0.5Cu Bal- 0.05 0.10 0.50 0.03 0.002 0.02 0.002 0.03 0.002 4.00 0.01
Sn-37Pb 62–64 Bal- 0.10 0.03 0.03 0.002 0.02 0.002 0.03 0.002 0.002 0.01
Sn-4Ag-0.5Cu Bal- 0.05 0.10 0.50 0.03 0.002 0.02 0.002 0.03 0.002 4.00 0.01
Metals 2019, 9, 209 3 of 10
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Table 2. The experimental condition and material melting point temperature.

MaterialTable 2. The experimental condition and material melting point temperature.

SPCT Method
Table 2. The experimental condition and material melting point temperature.
Material Reflow Condition SPCT Method
Melting Point SPCT Temp Aging Time (h) and
Solder Joint Material Reflow TempReflowReflow
Condition
Time SPCT Method
Temp (°C) Point
Melting (°C)
SPCT Temp Temp Time
Aging (°C) (h) and
Solder Joint (°C) Temp Reflow Condition
(s)
Melting Reflow
Point Temp Reflow Time SPCT Temp Aging Time(°C)
(h)
Solder Joint Temp (°C) Reflow Temp Reflow (°C) Temp
Sn-37Pb 183 (◦ C) (°C)
200 (±5) ◦
(s) Time (◦ C) and Temp (◦ C)
( C) 30 (s) 30 0, 200, 600 (At 150 °C)
Sn-4Ag-0.5Cu
Sn-37Pb 223 183 240 (±5)
200 (±5)
Sn-37Pb 183 200 (±5) 30 30 30 30 0, 200,
0, 200, 600600(At
(At150 °C)
Sn-4Ag-0.5Cu
Sn-4Ag-0.5Cu 223 223 240 (±5)
240 (±5) 150 ◦ C)
2.2. Experimental Method and Conditions
2.2.
2.2. Experimental
Experimental
Figure Method
2 shows Method and Conditions
and Conditions
the schematic diagram of the experimental setup for the SPCT method and the
deformationFigure
Figure of 2the solder
2 shows
shows thejoint
the during diagram
schematic
schematic applied
diagramstress. theFigure
of the
of 3a shows
experimental
experimental the for
setup
setup photo theof
for the the experimental
SPCT
SPCT method and
method and the
the
setup for the SPCT
deformation
deformation equipment,
of the
of the solder joint
solder andduring
joint Figureapplied
during 3b shows
applied the enlarged
stress.
stress. Figure 3a
Figure 3aview
shows
shows of the
the photo
photo of of the
the experimental
specimen
experimental
setup
setup for the SPCT equipment, and Figure 3b shows the enlarged view of the photo of thecrucial
device.
setup for Figure
the SPCT 2a shows
equipment, a schematic
and diagram
Figure 3b of
shows the whole
the SPCT
enlarged composed
view of the system.
photo ofThe
the specimen
specimen
devices of SPCT
setupdevice.
setup are
device. Figure composed
Figure 2a 2a shows of the lower
shows aa schematic and
schematic diagram upper
diagramof die,
of the furnace,
the whole
whole SPCT control
SPCT composed panel,
composedsystem. linear
system. Thevariable
The crucial
crucial
differential
devices transformer
of SPCT are (LVDT),
composed loading
of system
the lower and
and computer.
upper Figure
die, 2b
furnace,
devices of SPCT are composed of the lower and upper die, furnace, control panel, linear variable shows
controlthe lower
panel, and
linearupper
variable
die differential
used to clamp
differential the specimen
transformer
transformer (LVDT),and loading
(LVDT), to applysystem
loading a load on
system the
and
and punch. The
computer.
computer. creep
Figure
Figure 2bdisplacement-time
2b showsthe
shows thelower
lowerand curve
and upper
upper
behavior
dieused
die of both
used to solder
to clamp
clamp the joints
the specimen exhibits
specimenand the
andto same
to apply typical
apply aa load stages
load on
on the as those
the punch.
punch. The found
The creep in previous research
creep displacement-time
displacement-time curve on
curve
conventional
behavior creep
of both tests,
solder such as
joints primary,
exhibits secondary
the same and
typical tertiary
stages stages
as those[10]. According
found
behavior of both solder joints exhibits the same typical stages as those found in previous research on in to
previous Figure 2b,
research on
many stresses
conventional (i.e.,
creepcompressive,
tests, such tensile,
as primary,and shear
secondarystress)
and were found
tertiary in
stages
conventional creep tests, such as primary, secondary and tertiary stages [10]. According to Figure 2b, Region
[10]. A. However,
According to the
Figure 2b,
fractures
manywere
many stressesmostly
stresses (i.e.,generated
(i.e., compressive,
compressive, by shear stress
tensile,
tensile, and
andfollowed
shear by both
shear stress)
stress) compressive
were
were found in
found inand tensile
Region
Region A. stresses
A. However,
However, on the
the
the fractures
solder
fracturesjoints.
were mostly generated by shear stress followed by both compressive
were mostly generated by shear stress followed by both compressive and tensile stresses on and tensile stresses on
the solder
the solderjoints.
joints.

(a) SPCT equipment (b) die assembly

(a) SPCT of
Figure 2. Schematic diagram equipment (b) die
the experimental setup for the shear assembly
punch creep test and the
deformation of the solder
Figure 2.2. Schematic
Figure joint
Schematic diagram during applied stress.
diagram of the experimental setup for the shear punch
punch creep
creep test
test and
and the
the
deformationof
deformation ofthe
thesolder
solderjoint
jointduring
duringapplied
appliedstress.
stress.

(a) Photo of SPCT equipment (b) Enlarge view of specimen setup device
(a)Figure
Photo
Figure
of SPCT
3. Photo
3. Photo
equipment
of the
of experimental setup
the experimental
(b)for
Enlarge
for the
setup shear
view
punch
the shear
of specimen
creep
punch test.test.
creep
setup device
Figure 3. Photo of the experimental setup for the shear punch creep test.
Metals2019,
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Hence, the main stress applied to the specimens is the average shear stress (τ), as shown in the
Hence,equation
following the main stress applied to the specimens is the average shear stress (τ), as shown in the
[11]:
following equation [11]:
PP
τ τ== (1)
(1)
πdt
πdt
wherePP==punch
where load,t t==thickness
punchload, thicknessofofthe specimen,dd==average
thespecimen, averageofofdd1 1and
anddd22(d
(d22 is
is the
the diameter
diameter of ofthe
the
punch and d
punch (Ø2.8 mm), and d1 is the diameter of the Cu substrate hold (Ø3.2 mm)). The shear strain (ε)
(Ø2.8 mm), 1 is the diameter of the Cu substrate hold (Ø3.2 mm)). The shear strain (ε)
shown
shown in
in Figure
Figure2a
2a(Region
(Region A) A)was
wasobtained
obtained using
using the
the following
following equation
equation [12].
[12]. Here,
Here, δδ is
is the
the creep
creep
displacement
displacementthat
thatoccurs
occursduring
duringcreep
creepdeformation.
deformation.
δδ
ε=
ε= (2)
(2)
(d(d1 −− dd2 ))/2
2
1 2

Figure
Figure 44 shows
shows the preparation of
the preparation of aa schematic
schematicview
viewofofthe
thecross-section
cross-sectionspecimen
specimenonon Region
Region B.
B.
Meanwhile, to analyze the IMC behavior, the cross-section of the specimen was mounted to aa
Meanwhile, to analyze the IMC behavior, the cross-section of the specimen was mounted to
thermosetting
thermosetting resin
resin and
and polished
polished with
with sandpaper
sandpaper andand 0.05
0.05 micro
microaluminum
aluminumpowders.
powders. Finally,
Finally, the
the
interface
interfaceofofthe mounted
the mounted solder jointjoint
solder specimens was etched
specimens for 15 sfor
was etched using
15 as solution
using a (93 mL of methanol,
solution (93 ml of
2methanol,
mL of HCl andof5HCl
2 ml mL and
of NHO
5 ml3 ).
ofAfter
NHOthat, Thethat,
3). After IMCThe
behavior at the interface
IMC behavior of the cross-section
at the interface of the cross-
specimens (Region (Region
section specimens B) was investigated using SEM
B) was investigated andSEM
using EDS.and EDS.

Figure4.
Figure 4. Schematic
Schematic view
view of
ofthe
the cross-section
cross-sectionspecimen
specimenon
onregion
regionB.
B.

3.
3. Result
Result and
and Discussion
Discussion

3.1. SPCT Displacement-Time Curve

3.1. SPCT Displacement-Time Curve
The creep data obtained from the SPCT method for different aging times is shown in
The creep data obtained from the SPCT method for different aging times is shown in Figures 5
Figures 5 and 6. The creep displacement-time curves of the Sn-37Pb and Sn-4Ag-0.5Cu solder joints
and 6. The creep displacement-time curves of the Sn-37Pb and Sn-4Ag-0.5Cu solder joints are shown
are shown in Figures 5 and 6, respectively. The creep curve behavior exhibits the primary, secondary
in Figures 5 and 6, respectively. The creep curve behavior exhibits the primary, secondary and tertiary
and tertiary stages. It can be seen that the overall creep curves are significantly different from each
stages. It can be seen that the overall creep curves are significantly different from each other according
other according to the aging time and applied load. One can also see that the rupture time significantly
to the aging time and applied load. One can also see that the rupture time significantly decreases with
decreases with the increase of aging time and applied load. This can be explained due to the brittleness
the increase of aging time and applied load. This can be explained due to the brittleness of solder
of solder joints and the matrix grain coarsening of IMC that occurred on the interface between the
joints and the matrix grain coarsening of IMC that occurred on the interface between the solder joint
solder joint and Cu substrates after isothermal aging, thus decreasing the bonding strength between
and Cu substrates after isothermal aging, thus decreasing the bonding strength between the solder
the solder joint and Cu substrates. In the case of applied loads 49 N and 53.9 N, the displacements (δ)
joint and Cu substrates. In the case of applied loads 49 N and 53.9 N, the displacements (δ) of the
of the curves are higher than for other conditions (see Figure 5b,c). Because the solder joints have a
curves are higher than for other conditions (see Figure 5b,c). Because the solder joints have a higher
higher elongation property than for other aging time conditions (200 h and 600 h), the ductile fractures
elongation property than for other aging time conditions (200 h and 600 h), the ductile fractures were
were predicted to occur in this case.
predicted to occur in this case.
Metals 2019, 9, 209 5 of 10
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0.8
0.8
(a) (b)
(a) (b)
Displacement,δ(mm)
0.7 0.4
Displacement,δ(mm) 0.7 0.4

δ(mm)
68.6N 53.9N

Displacement,δ(mm)
68.6N 53.9N 49N
0.5 58.8N 49N
0.5 58.8N 53.9N 39.2N
0.3 53.9N 39.2N 34.3N
0.4 0.3 49N 34.3N

Displacement,
0.4 49N
0.3
0.3 0.1
0.1
0.1
0.1
0.0 0
0.0 0 10 20 30 40 50 00 10 20 30 40 50 60 70
0 10 20 30 40 50 0 10 20 30 Time,
40 t(h)50 60 70
Time, t(h) Time, t(h)
Time, t(h)
0.5
0.5
(c)
δ(mm)

(c)
Displacement,δ(mm)

0.4
0.4

0.3 39.2 31.8N

Displacement,

0.3 39.2 31.8N 29.4N

24.5N
29.4N 24.5N
0.2
0.2

0.1
0.1

0
00 5 10 15 20 25 30
0 5 10 Time,
15 t(h) 20 25 30
Time, t(h)
Figure 5. Displacement-time curves for Sn-37Pb for different aging times (a) 0 h, (b) 200 h, and (c) 600 h.
Figure 5.5.Displacement-time
Figure curvesfor
Displacement-time curves forSn-37Pb
Sn-37Pbfor
fordifferent
different aging
aging times
times (a) 0(a)
h,0(b)
h, 200
(b) 200 h, and
h, and (c)h.600 h.
(c) 600

1.25 0.8
1.25 0.8
(a) 0.7 63.7N (b)
(a) 0.7 63.7N (b)
δ(mm)

δ(mm)

1
Displacement,δ(mm)

Displacement,δ(mm)

1 0.6
0.6 61.2N
93.1N 61.2N
0.75 93.1N 0.5 49N
78.4N 0.5 49N
0.75 88.2N 83.3N 78.4N 58.5N
Displacement,

Displacement,

88.2N 83.3N 0.4 58.5N

0.4
0.5 0.3
0.5 0.3
0.2
0.25 0.2
0.25 0.1
0.1
0 0
0 0 20 40 60 80 0 0 5 10 15 20 25 30
0 20 40 t(h)
Time, 60 80 0 5 10 Time,
15 t(h) 20 25 30
Time, t(h) Time, t(h)
0.8
0.8
(c)
(c)
0.7
δ(mm)

0.7
Displacement,δ(mm)

0.6
0.6
0.5 58.8N 46.5N
Displacement,

0.5 58.8N 51.4N 44.1N

46.5N 44.1N
51.4N
0.3
0.3
0.2
0.2
0.1
0.1
0
00 10 20 30 40
0 10 20 30 40
Time,
Time, t(h)
t(h)
Figure Displacement-time
Figure 6. Displacement-time curves
curves for Sn-4Ag-0.5Cu
for Sn-4Ag-0.5Cu for different
for different aging
aging time (a) 0time (a)200
h, (b) 0 h, and
(b) 200 h, and
(c) 600 h.
Figure 6. Displacement-time curves for Sn-4Ag-0.5Cu for different aging time (a) 0 h, (b) 200 h, and (c) 600 h.
(c) 600 h.
3.2. Power-Law Relationship
3.2. Power-Law Relationship
3.2. Power-Law Relationship
Figure 7 shows the power-law relationship between the rupture time of the solder joint (tr ) and
the average shear stress (τ) for the SPCT method. Figure 6 shows that the creep rupture time of the
Metals 2019, 9, 209 6 of 10

MetalsFigure 7 shows the power-law relationship between the rupture time of the solder joint (tr)6 and
2019, 9, 209 of 10
the average shear stress (τ) for the SPCT method. Figure 6 shows that the creep rupture time of the
solder joint decreased with an increase of the punch pressure. Equation (3) is a general power law
solder joint decreased
relationship [13]: with an increase of the punch pressure. Equation (3) is a general power law
relationship [13]:
Aτ−−nn
trtr== Aτ (3)
(3)

where, A = = material constant, ττ = average shear stress, n == stress exponent. Generally, the stress
exponent. Generally,
exponent (n) decreased with an increase
increase of the aging time (see Figure 7). This can be explained by the
behavior of
of the
theIMC,
IMC,which
whichchanged
changedwith withananincrease
increase in in
thethe
aging
agingtime. This
time. causes
This thethe
causes strength of the
strength of
solder
the joint
solder to get
joint weaker.
to get The
weaker. mean
The mean thickness
thickness of of
the interfacial
the interfacialCu 5 Zn
Cu 5Zn8 8IMC
IMClayers
layersin
in the
the specimen
increased with an increase in the the thermal
thermal aging
aging time,
time, following
following aa parabolic
parabolic lawlaw [14].
[14]. The stress
Sn-37Pb at
exponent (n) of the Pb-free solder joints is higher than Sn-37Pb at the
the same
same temperature.
temperature. Commonly,
Commonly,
the creep life of Pb-free Sn-4Ag-0.5Cu solder joints
joints are
are longer
longer than
than that
that of
of Sn-37Pb
Sn-37Pb solder
solder joints.
joints.

3
10

2
10
Rupture time, tr(h)

1
10

0
10

-1
10
n =6.1 n =11.6
Sn-37Pb-600h Sn-4Ag-0.5Cu-600h
-2
10 n
Sn-37Pb-200h
=9.2 n
Sn-4Ag-0.5Cu-200h
=17.5
n =12.75 n =18.49
Sn-37Pb-0h Sn-4Ag-0.5Cu-0h
-3
10
4 5 6 7 8 9 10 20
Applied Stress, τ(M Pa)
Figure 7.
Figure Power law
7. Power law relationships
relationships for
for both
both aged
aged solders
solders joints.
joints.

The creep rupture time (t ) of the solder joints with the aging time was calculated using the
The creep rupture time (trr) of the solder joints with the aging time was calculated using the
following power law relationship equation:
following power law relationship equation:
The power law relationship equation of Sn-37Pb and Sn-4Ag-0.5Cu solder joints:
The power law relationship equation of Sn-37Pb and Sn-4Ag-0.5Cu solder joints:
- Sn-37Pb solder joint Sn-4Ag-0.5Cu solder joint
- Sn-37Pb solder joint
−12.75
Sn-4Ag-0.5Cu solder joint
-Aging 0 -Aging
h tr = 4.48 × 10 ⋅ τ
14
− tr = 2.75 × 1024 ⋅ τ −18.49
0h tr = 4.48 × 10 · τ 14 12.75 tr = 2.75 × 1024 · τ−18.49
−9.2 −17.5 (4)
(4)
-Aging 200 h 200trh= 7.4 × 10tr ⋅=
-Aging
9
τ 7.4 × 10 · τ9 − 9.2 tr =tr1.78 × 1020×⋅ τ10
= 1.78 20 · τ−17.5

h 600trh= 9.94 ×t10

-Aging
-Aging 600 r =⋅ τ
5 −6.1
9.94 × 105 · τ−6.1 tr =tr7.49= 7.49 12 · τ−11.6
−11.6
× 1012×⋅ τ10

3.3. Monkman-Grant
3.3. Monkman-Grant Relationship
Relationship
The Monkman-Grant
The Monkman-Grantrelational
relationalequation
equationisiswidely
widely used
used in inthethe creep
creep failure
failure modeling.
modeling. It hasIt also
has
also been used to evaluate this experiment to predict
been used to evaluate this experiment to predict the creep rupture the creep rupture time [15]. This relationship
time [15]. This relationship is
.
is obtained
obtained from
from thethe relationship
relationship between
between thethe
creepcreep strain
strain raterate
( ε )(ε)
and andthethe creep
creep rupture
rupture timetime
(tr),(tas
r ),
as follows.
follows. .m
tr ε = b (5)
trε m = b (5)
where, tr = fracture time, m = Monkman-Grant exponent, b = material constant. The slope of the
relationship
Where, plot is approximately
tr = fracture 1 and indicatesexponent,
time, m = Monkman-Grant that it is valid for the SPCT
b = material method
constant. The[16].
slope Figure
of the 8
shows that the
relationship Monkman-Grant
plot is approximatelyrelationship of both
1 and indicates thatsolder jointsfor
it is valid inthe
relation
SPCTtomethod
the creep strain
[16]. Figurerate8
.
(shows
ε) andthat
the the
creep rupture time (trrelationship
Monkman-Grant ) for different
of aging times.joints
both solder The Monkman-Grant exponents
in relation to the creep strain(m)rateof(
ε ) and
the solder
thejoints
creepare 0.71 and
rupture time1.1,(twhich is close to
r) for different 1. This
aging means
times. Thethat the SPCT method
Monkman-Grant applies (m)
exponents in theof
the solder joints are 0.71 and 1.1, which is close to 1. This means that the SPCT method applies in the
Metals 2019, 9, 209 7 of 10
Metals 2019, 9, 209 7 of 10

assessment of the creep mechanical properties of both the conventional and the Pb-free solder joints.
assessment of the creep mechanical properties of both the conventional and the Pb-free solder joints.
The Monkman-Grant relationship of each solder joint is as follows:
The Monkman-Grant relationship of each solder joint is as follows:
. 0.71
Sn-37Pb:t
Sn-37Pb: ε = 0.18
trεr0.71 = 0.18
. 1.1 (6)
(6)
Sn-4Ag-0.5Cu: rtεε 1.1 =
Sn-4Ag-0.5Cu:t = 0.03
0.03
r

3 3
10 10
(a) aging 0h (b) Aging 0h
Aging 200h Aging 200h
2
Aging 600h
Rupture time, tr(h)

2
10 10 Aging 600h

Rupture time, tr(h)

1 1
10 10

0 0
10 10

-1 -1
10 10
-4 -3 -2 -1 0 1
10 10 10 10 10 10 10
-4 -3
10 10
-2
10
-1
10
0
10
1

Creep Strain Rate, ε (h )

-1
Creep Strain Rate, ε (h )
o o
-1

Figure 8. Monkman-Grant relationship of (a) Sn-37Pb and (b) Sn-4Ag-0.5Cu.

3.4. Observation of IMC Behavior

We also investigated the IMC formation during the high-temperature reflow process in order
to assess and evaluate the properties of the solder joints. However, the overgrowth of IMC leads to
brittleness, which causes brittle fracture and the deterioration of the bonding strength between the
solder joint and substrate. As a result, the observation of the IMC formation is an essential factor for
solder joints [9,17]. Figures 9 and 10 show the phase and morphology of IMC of each solder joint
using SEM and EDS after aging at 150 ◦ C for 0, 200, and 600 h respectively. The results obtained from
Figures 9 and 10 show that for both solders the thickness of the IMC layer at the Cu interface gradually
increases with the aging time. The IMC morphology changed significantly from a stable to irregular
state and from a small round to long needle-like shape when the aging time increased. Figure 9 shows
the IMC Ni3 Sn4Figure 8. Monkman-Grant
, Sn-rich, and Pb-rich phasesrelationship of (a)
for 0 and 200Sn-37Pb andIn
h aging. (b)addition,
Sn-4Ag-0.5Cu.
voids and other IMC
phases (Cu, Ni)6 Sn5 were observed at 600 h. This changed behavior of the IMC at the Cu interface
3.4. Observation
shows of IMC
that the initial Behavioris gradually evolving to brittleness with increasing aging time. Figure 10
ductility
showsWethat
alsothe IMC phasethe
investigated (Cu,
IMCNi)formation
6 Sn5 , Ni3 Sn 4 wasthe
during observed from an aging
high-temperature timeprocess
reflow of 200 h,
in and that
order to
the voids appeared for an aging time of 600 h. Overall, the IMC interface of the Sn-4Ag-0.5Cu
assess and evaluate the properties of the solder joints. However, the overgrowth of IMC leads to solder
joints was found
brittleness, whichtocauses
be more stable
brittle than that
fracture andofthe
thedeterioration
Sn-37Pb solder.
of the bonding strength between the
solder joint and substrate. As a result, the observation of the IMC formation is an essential factor for
solder joints [9,17]. Figures 9 and 10 show the phase and morphology of IMC of each solder joint
using SEM and EDS after aging at 150 °C for 0, 200, and 600 h respectively. The results obtained from
Figures 9 and 10 show that for both solders the thickness of the IMC layer at the Cu interface
gradually increases with the aging time. The IMC morphology changed significantly from a stable to
irregular state and from a small round to long needle-like shape when the aging time increased.
Figure 9 shows the IMC Ni3Sn4, Sn-rich, and Pb-rich phases for 0 and 200 h aging. In addition, voids
and other IMC phases (Cu, Ni)6Sn5 were observed at 600 h. This changed behavior of the IMC at the
Cu interface shows that the initial ductility is gradually evolving to brittleness with increasing aging
time. Figure 10 shows that the IMC phase (Cu, Ni)6Sn5, Ni3Sn4 was observed from an aging time of
200 h, and that the voids appeared for an aging time of 600 h. Overall, the IMC interface of the Sn-
4Ag-0.5Cu solder joints was found to be more stable than that of the Sn-37Pb solder.
 Metals 2019, 9, 209 8 of 10

Metals 2019, 9,
Metals 2019, 9, 209
209 88 of 10
10

Ni3Sn4 Pb-rich Sn-rich

Ni3Sn4 Pb-rich Sn-rich

Ni-P layer
Cu
Ni-P layer
(a)
Cu
(a)

Figure
Figure 9. SEM
9. SEM images
images of Sn-37Pb
of Sn-37Pb after
after aging
aging timetime
(a) 0(a)
h,0(b)
h, 200
(b) 200 h, and
h, and (c) 600
(c) 600 h. h.

Figure 9. SEM images of Sn-37Pb after aging time (a) 0 h, (b) 200 h, and (c) 600 h.

Figure 10. SEM images of Sn-4Ag-0.5Cu after aging time (a) 0 h, (b) 200 h, (c) and 600 h.

4. Conclusions
Figure 10. SEM images of Sn-4Ag-0.5Cu after aging time (a) 0 h, (b) 200 h, (c) and 600 h.

In thisFigure
research, we evaluated the creep mechanical properties of Sn-37Pb and Sn-4Ag-0.5Cu
10. SEM images of Sn-4Ag-0.5Cu after aging time (a) 0 h, (b) 200 h, (c) and 600 h.
4. Conclusion
solder joints for different aging times (0, 200, 600 h) by investigating IMC behavior and using the SPCT
method. InThe
this
4. Conclusion research, we
conclusions evaluated
of this study arethesummarized
creep mechanical properties of Sn-37Pb and Sn-4Ag-0.5Cu
as follows.
solder joints for different aging times (0, 200, 600 h) by investigating IMC behavior and using the
1. Based
In this on the results
research, of the SEM the
micro images, the thickness of theofIMC increased,
and and the shape
SPCT method. The we evaluated
conclusions of thiscreep
studymechanical properties
are summarized Sn-37Pb
as follows. Sn-4Ag-0.5Cu
solder joints for different aging times (0, 200, 600 h) by investigating IMC behavior and usingtime.
of the IMC morphologies changed from round to needle-like with an increase of the aging the
After isothermal aging (200 and 600 h), the IMC (Cu,
SPCT method. The conclusions of this study are summarized as follows. Ni) 6 Sn 5 phases and the micro voids were
Metals 2019, 9, 209 9 of 10

found on the solder joint/Cu substrate interface. This means that the brittleness of the solder
increased, thus causing the deterioration of mechanical properties.
2. The power-law relationship indicated that the stress exponent (n) and creep properties of
solder joints decreased with the increase of aging time, and that the values (n) of Sn-4Ag-0.5Cu
solder joints are higher than those of Sn-37Pb solder joints. It can thus be confirmed that the
creep properties of Sn-4Ag-0.5Cu solder joints are better than those of conventional Sn-37Pb
solder joints.
3. The Monkman-Grant relationship shows that the exponent value (m) solder joints are close to
1. It can thus be confirmed that the SPCT method is a reliable method, which can be used to
evaluate the creep properties of solder joints.
4. Based on our results, the obtained mechanical properties of Pb-free Sn-4Ag-0.5Cu solder joints
are greater than those of Sn-37Pb solder joints for all isothermal aging time conditions (0, 200,
600 h). In addition, the melting point temperature of Sn-4Ag-0.5Cu solder joints is similar to that
of conventional Sn-37Pb solder joints. Therefore, it is possible to use Pb-free Sn-4Ag-0.5Cu solder
joints in electrical applications, rather than Sn-37Pb solder joints.

Author Contributions: Conceptualization, S.H. and H.S.Y.; methodology, S.H.; software, S.H.; formal analysis, S.H.
and H.S.Y.; investigation, H.S.Y.; data curation, S.H.; writing—original draft preparation, S.H.; writing—review
and editing, H.S.Y.
Funding: This work was supported by Chonbuk National University, the Republic of Korea in 2018.
Conflicts of Interest: The authors have no conflict of interest to declare.

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