Properties of Lead Free Solder Alloys as a Function of Composition

Variation
Qing Wang(1) , William F.Gale(2), R. Wayne Johnson(1), David Lindahl(2)
and Hongtao Ma(1)
Laboratory for Electronics Assembly & Packaging Auburn University
(1) Electrical Engineering Department
162 Broun Hall
Auburn, AL 36849 USA
334-844-1880
johnson@eng.auburn.edu
(2) Materials Research and Education Center

Abstract
While the electronics industry appears to be converging on Sn-Ag-Cu as the alloy of choice for lead free
electronics assembly, the exact composition varies by geographic region, supplier and user. Add to that
dissolved copper and silver from the printed circuit board traces and surface finish, and there can be
significant variation in the final solder joint composition. This paper presents the results of a systematic
study of the mechanical and microstructural properties of Sn-Ag-Cu alloys with Ag varying from 2wt% to
4wt% and Cu varying from 0.5wt% to 1.5wt%.
Different sample preparation techniques (water quenched, oil quenched and water quenched followed by
reflow) were explored and the resulting microstructure was compared to that of a typical reflowed lead free
chip scale package (CSP) solder joint. The microstructure obtained by oil quenching produced a
microstructure similar to that of the CSP solder joint. The water quenched sample had a finer grain
structure, while the water quenched and reflowed sample had a coarser grain structure compared to the CSP
solder joint. The sample preparation technique and comparative microstructures are presented.
The tensile strength, 0.2% yield strength and the ultimate tensile strength have been measured for the range
of alloys at conditions of as-cast, aged for 100h at 125oC and aged for 250h at 125oC. The creep test results
and the effect of high temperature aging on mechanical properties are also presented for the oil quenched
samples.
The results of this work provide necessary data for the modeling of solder joint reliability for a range of SnAg-Cu compositions and a baseline for evaluating the effects of subsequent quaternary additions.
Introduction
Lead free solders have seen increasing use in interconnection systems for electronic packages due to
pending legislation in the European Union, environmental and health concerns, and market competition.
The European Commissions (EC) draft directives, Waste Electrical and Electronic Equipment (WEEE)
and Restriction of Hazardous Substances (Rohs), have approved the ban of Pb in electronics effective July
2006 in European Union countries. Furthermore, several Japanese electronics manufacturers have
successfully created a market differentiation and increased market share based on green products that use
Pb-free solders. The conversion to Pb-free solders in the electronics assembly appears imminent [1].
A large number of lead free solder research studies [2-7] have been reported which have focused on
microstructural analysis, tensile properties including Youngs modulus, Poissons ratio, tensile strength,
creep properties for specified compositions of lead free solders. According to the research report [4] of the
National Center for Manufacturing Science (NCMS) and the National Electronics Manufacturing Initiative
(NEMI), there is no drop in replacement for SnPb eutectic solder. Sn-Ag-Cu alloy has been proposed as
the main option for lead free solder in reflow applications due to its relatively low melting temperature, as
well as its superior mechanical properties and solderability compared with other lead free solders.

While the electronics industry appears to be converging on Sn-Ag-Cu as the alloy of choice for lead free
electronics assembly, the exact composition varies by geographic region, supplier and user. Add to that
dissolved copper and silver from the printed circuit board traces and surface finish, and there can be
significant variation in final solder joint composition. Current research reports have not provided a
systematic study of Sn-Ag-Cu lead free solder as a function of alloy composition. The dimensions of the
specimens used were not close to those of real solder joints in electronic packages such as BGAs and
CSPs. This will significantly affect the microstructure of the sample, as well as the mechanical properties.
Also, there is little experimental data available on the effect of aging on the mechanical properties
including creep and tensile behavior for the wide range of Sn-Ag-Cu ternary alloys.
In this study, a new fabrication technique which produces specimens with microstructure very similar to a
real CSP solder joint was developed to systematic study the mechanical and microstructural properties of
Sn-Ag-Cu alloys with Ag varying from 2wt% to 4wt% and Cu varying from 0.5wt% to 1.5wt%. Tensile
and creep properties, as well as the effects of aging on these properties for a selected range of alloy
compositions are reported.
Specimen Preparation
The solder alloy compositions investigated in this study covered Ag from 2.0~4.0 % and Cu from 0.5~1.5%
by weight percent. Sn is the base metal of the alloy. In the specimen preparation process, commercial tin
shot (purity 99.99 +%, 3mm), silver shot (99.9 +%, 1-5mm) and copper shot (99.5+%, 0.5-0.8mm) were
mixed according to the specified composition ratio (Table 1), and then mixed with small quantities of flux
(Kester Tacky Flux TSF-6522). The alloy mixture was put in a fused-quartz crucible and heated on a hot
plate. The melting process was performed in an inert environment (vacuum was first applied and then the
sample was purged with argon gas). The heating profile is shown in Figure 1. Table 1 shows the chemical
composition of solder alloys measured by Plasma Emission Spectroscopy.

Figure 1- Heating Profile for Alloy Melting

Alloy
Chemical
Composition

Table 1-Target Alloy Composition Matrix and Chemical Analysis

Target Ag (wt.%)
4%

1.5% 94.7Sn3.9Ag1.4Cu

3.5%

3.0%

95.2Sn3.4Ag1.4Cu

95.6Sn3Ag1.4Cu

2.5%

2.0%

96.23Sn2.47Ag1.4Cu 96.58Sn2.02Ag1.4Cu

Target 1.2% 94.7Sn4.06Ag1.24Cu 95.2Sn3.6Ag1.2Cu 95.78Sn3Ag1.22Cu 96.44Sn2.4Ag1.16Cu 96.86S2.01Ag1.13Cu

Cu
95.23Sn3.92Ag0.85Cu 95.64Sn3.5Ag0.86Cu 96.28Sn2.9Ag0.82Cu 96.6Sn2.5Ag0.8Cu 97.28Sn2.02Ag0.8Cu
(wt.%) 0.8%
0.5% 95.52Sn4.0Ag0.51Cu 96.06Sn3.4Ag0.54Cu 96.47Sn2.9Ag0.53Cu 96.96Sn2.55Ag0.49Cu 97.46Sn2.04Ag0.5Cu
Actual chemical analysis shown in table compared to target composition indicated by row and column
headings.

An advanced specimen preparation process was developed using rectangular cross-section small glass tubes
and a controlled vacuum system (Figure 2). The solder was melted in a quartz crucible (L=120mm,
=19mm) with a heating coil. A thermocouple and temperature control module was used to monitor and
control the melting process temperature. After the temperature of the molten solder had maintained the
desired temperature for 5 minutes, the glass tube connected to the controlled vacuum system was inserted
into the molten solder and the solder was sucked into the glass tube. The glass tube was immersed in oil or
cold water immediately after filling. Once the sample cooled to room temperature, the specimen could be
extracted due to the lower CTE of the glass compared to the solder (Figure 2). Figure 3 shows the
dimension of the specimen made by this process [8]. Compared with the dog-bone or casting specimens
used by other researchers [2-5], the thickness of the Auburn uni-axial specimen is close to that of real CSP
(0.25~0.5mm) and BGA (0.5mm) solder joints.

(a) Solder Melting System

(b) Specimen solidified in glass tube

(c) Specimen after removal from glass tube

Figure 2 - Solder Melting System and Specimen Preparation [8]

Figure 3 - Auburn Uni-axial Specimen [8]

Microstructure of the SnAgCu System

The mechanical properties of alloy specimens depend on their microstructure. Hence the challenge is to
make a specimen which has a comparable microstructure to a real solder joint. The microstructure is
controlled by the cooling profile. In this study, cooling options were: oil quench; water quench; and water
quench followed by a 248oC peak reflow in a Heller 1800 reflow furnace (Figure 4). The resulting
microstructure was compared with a CSP solder joint (95.5Sn4Ag0.5Cu) reflowed using the CSP quick
ramp profile (Figure 4)

Reflow profile (Peak temp = 248C)

CSP quick ramp reflow (peak temp=245 C)

Figure 4 - Specimen Cooling Options and CSP Reflow Profile

Specimens with the different cooling options were polished with SiC papers, diamond paste and finally
with Al2O3 paste to a 0.1 micrometer finish. All samples were etched for a few seconds with 5% volume of
hydrochloric acid in methanol. A scanning electron microscope (SEM) was used to analyze the
microstructure.
Figure 5 compares the SEM microstructures (95.5Sn4Ag0.5Cu) from the different cooling conditions with
the CSP solder joint. With the aid of energy dispersion x-ray analysis (EDS), it is found that the dark areas
are a Sn rich phase and the bright areas, which are needle-like, elongated or spherical, are the Ag3Sn
intermetallic phase. Both the oil quenched specimen and CSP solder joint shown the eutectic region of Sn
and moderately dispersed Ag3Sn intermetallic surrounded by a dentritic Sn-rich phase. The microstructure
of the water quenched specimen consists of a mixture of eutectic regions of dense Ag3Sn intermetallic
within a tin rich matrix surrounding large equiaxed crystals of tin-rich solid solution [9]. The specimen
made by water quenching followed by a reflow cycle has a more coarse tin eutectic structure with irregular
dispersed Ag3Sn intermetallic precipitates. Based on the microstructure evaluation, the water quenched
specimen shown has a more fine microstructure than the CSP solder joint, while the specimen that was
water-quenched followed by reflow cycle showed a more coarse microstructure than the CSP solder joint.
The specimen prepared by oil quenching had a microstructure close to that of the CSP solder joint after
reflow. Based on these results, oil quenching was selected for fabrication of specimens for the tensile and
creep tests in the following section.
Tensile Properties of the SnAgCu System
Tensile tests were performed with an MT-200 tension/torsion thermo-mechanical test system made by
Wisdom Technology Inc. shown in Figure 6. The system provides an axial displacement resolution of 0.1
micrometer and a rotation resolution of 0.001o. The testing machine is under displacement control. Load
and displacement data were recorded and used to determine the true stress/true strain curve. True stress and
true strain were calculated from the engineering stress and strain by the conventional constant volume
assumption. Figure 7 indicates the Youngs modulus, 0.2%-strain yield stress and ultimate tensile strength
on a typical strain-stress testing curve measured at a strain rate of 10-3 (1/sec) at 25oC.

Figure 5 -Microstructure comparison between CSP Solder Joint and Specimens with Different
Cooling Options

Figure 6 - Micro Tension Tester

Figure 7 - Stress-strain Tensile Curve for 96.5Sn-3.5Ag-1.5Cu

A group of stress-strain tensile test curves for 96.5Sn-3.5Ag-1.5Cu is shown in Figure 8 to represent the
general test results. At least five specimens were tested for each alloy composition at each test condition.
Figure 8 shows that the tensile test data fits well with the elastoplastic model for 96.5Sn-3.5Ag-1.5Cu. The
elastoplastic model of lead free solder exhibits an elastic phase until a critical stress is reached (the yield
point), after which plastic behavior becomes dominant. It is normally used to predict the deformation of the
alloy on the stress-stain curve.

Test Temp: 25 oC
Strain Rate: 0.001 s-1

(a) Tensile measurement curves

(b) Elastoplastic model
Figure 8-Stress - strain Tensile Curve for 96.5Sn-3.5Ag-1.5Cu
Youngs modulus, 0.2% strain yield stress and ultimate tensile strength were measured for all 20 selected
alloy compositions (Table 1) at three conditions (as-cast, aged for 100h at 125 oC, aged for 250h at 125 oC).
The distribution of tensile properties as a function of alloy composition and their change with aging time
are shown in Figures 9-11. Youngs modulus (Figure 9) as a function of alloy composition (Ag=2%~4%,
Cu=0.5%~1.5%) ranged from 37-41 GPa and decreased to 30-32 GPa after aging for 100 hours and 250
hours at 125oC. There is no significant difference in Youngs Modulus as a function of alloy compositions.
After the initial decrease in modulus after 100 hours at 125oC, there was insignificant change with further
aging.

Figure 9(a) - Distribution of Youngs Modulus as a Function of Alloy Composition (As-cast)

Figure 9(b) - Distribution of Youngs Modulus as a Function of Alloy Composition (125oC, 100h
Aging)

Figure 9(c) - Distribution of Youngs Modulus as a Function of Alloy Composition (125oC, 250h
Aging)
The distribution of 0.2% strain yield stress and ultimate tensile strength as a function of alloy composition
was more significant as compared to the variation in Youngs modulus. Both were significantly higher with
higher levels of silver and copper. The 0.2% strain yield stress was 56 MPa for the Sn-4Ag-1.5Cu alloy and
34 MPa for the Sn-2Ag-0.5Cu alloy. After 100h aging at 125oC, the 0.2% strain yield stress for these alloys
decreased to 32 and 23 MPa, respectively. The maximum ultimate tensile stress was (61 MPa) for the Sn4Ag-1.5Cu alloy and only 38 MPa for the Sn-2Ag-0.5Cu alloy (Figure 11(a)). After 100 hours of aging at
125oC, the ultimate tensile stress for these two alloys decreased to 37 and 27 MPa, respectively. The
absolute values of the yield stress and the ultimate tensile stress, as well as the difference between values
for the different alloy compositions decreases during the aging process. There is no significant change in
the 0.2% strain yield stress and the ultimate tensile stress distribution for the different alloys after 100hours
of aging at 125oC.

Figure 10(a) - Distribution of 0.2% Strain Yield Stress as a Function of Alloy Composition (As-cast)

Figure 10(b) - Distribution of 0.2% Strain Yield Stress as a Function of Alloy Composition (125oC,
100h Aging)

Figure10(c) - Distribution of 0.2% Strain Yield Stress as Function of Alloy Composition (125oC, 250h
Aging)

Figure 11(a) - Distribution of Ultimate Tensile Strength as a Function of Alloy Composition (As-cast)

Figure 11(b) - Distribution of Ultimate Tensile Strength as a Function of Alloy Composition (125oC,
100h Aging)

Figure 11(c) - Distribution of Ultimate Tensile Strength as a Function of Alloy Composition (125oC,
250h Aging)

Strain

Creep properties of selected lead free solders

The creep data available in the literature for Sn-Ag-Cu ternary alloys are very limited. This hinders reliable
predictions using finite element analysis of electronic assemblies [3]. The systematic analysis of creep
properties over a wide range of Sn-Ag-Cu ternary alloy compositions after thermal aging is very important
for FEM analysis. If the creep properties of the alloy changes as a function of storage time at elevated
temperature, this must be included in the model for accurate predictions. Furthermore, there is little data
available for strain rates less than 10-6/sec, stress levels less than 10 MPa and temperatures above 75 oC or
combinations thereof [4]. However, the creep data at these conditions are very important as they represent
the real stress conditions of solder joints in electronic assemblies in service. In this study, creep tests were
performed with an MT-200 tension/torsion thermo-mechanical test system for selected alloy compositions
(Sn-4Ag-1.5Cu, Sn-4Sg-0.5Cu, Sn-2Ag-1.5Cu, Sn-2Ag-0.5Cu, Sn-3.5Ag-0.8Cu) for three conditions: ascast; aged for 100 hours at 125oC; and aged for 250 hours at 125oC. The selection of Sn-4Ag-1.5Cu, Sn4Sg-0.5Cu, Sn-2Ag-1.5Cu, Sn-2Ag-0.5Cu represent the four corners of the alloy range previously
characterized for tensile properties, while the Sn-3.5Ag-0.8Cu represents a mid-point and is close to the
eutectic composition of the SnAgCu ternary alloy. Tests were conducted for three different temperatures
(22oC, 100oC and 150oC) at different constant stress levels. A thermal chamber was used for creep test at
different temperature. The temperature of the specimens was monitored and controlled by a thermocouple
placed close to the center of the specimen. The creep curves display typical primary creep, quasi-steady
state (constant strain rate) and tertiary rupture stages (Figure 12). The quasi-steady state is dominant in the
creep process. The creep strain rate was determined by differentiating the creep strain with respect to time.
Each test was continued until the minimum true strain rate was identified. The creep specimens will fail
earlier at high applied stress and have a long quasi-steady-state at low applied stress (Figure 13).

Quasi-steady state:
d/dt = constant

Rupture

Primary
Creep
Secondary creep

Tertiary
creep

Initial strain
(Elastic +plastic)

t (time)
Figure 12 - Conventional Steady Strain Rate Creep Curve [4]
As a benchmark, the authors data is compared with reported reference creep data [4] in Figure 14. It
shows the quasi-steady state creep rates plotted against applied stress in the log-log format. In general, the
creep data from these sources are in the same range even though the sample dimensions, sample
preparation and exact compositions vary (Table 2).

Figure 13 - Experimental Creep Curves for 94.5Sn-4Ag-1.5Cu (100h, 125oC Aging) at T=150oC at
Different Stress Levels

Figure 14 - Comparison of Creep Data [4]

Source
Auburn Univ.
Schubert et
Neu et
Karriya et

Table 2 - Comparison of Creep Specimens

Alloy Composition
Specimen
Specimen/Gauge Cross-section
shape
length
95.7Sn3.5Ag0.8Cu
Uni-axial
60mm/50~60mm 3mm x 0.5mm
rectangular
rectangular
95.5Sn3.8Ag0.7Cu
Dog-bone
60mm/30mm
3mm x 3mm
96.2Sn2.5Ag0.8Cu
Cylinder
127mm/12.7mm 13mm square
95.5Sn3.8Ag0.7Cu
Dog-bone
60mm gauge
11.28mm
96.5Sn3.0Ag0.5Cu
square

Specimen
treatment
Oil quench
Not reported
Air-cooled
Water
quenched

The creep curves for the five selected alloy compositions at the different aging conditions are shown in
Figures 15-17 for test temperatures of 22oC, 100oC and 150oC respectively. The creep curves shift from
right to left, indicating that the creep resistance decreases as the test temperature is increased for all five
alloy compositions. For each alloy composition, the creep resistance decreases as the aging time at 125oC
increases. Sn4Ag1.5Cu has the highest creep resistance and Sn3.5Ag0.5Cu ranks second. The creep
resistance for Sn2Ag0.5Cu, Sn4Ag0.5Cu and Sn2Ag1.5Cu are similar and lower.

Figure 15 - Comparison of Creep Data at T=22 oC (As-cast, and Aging 100h, Aging 250h at 125oC)

Figure 16 - Comparison of Creep Data at T=100oC (As-cast, and Aging 100h, Aging 250h at 125oC)

Figure 17 - Comparison of Creep Data at T=150oC (As-cast, and Aging 100h, Aging 250h at 125oC)

Creep constitutive models

The quasi-steady state creep constitutive model can be simply characterized by a power law relationship,
Q

 = A ne kT

(1)

where the quasi-steady state creep strain rate is , A is a material constant, is the applied stress, n is the
stress exponent, Q is the creep activation energy, k is Boltzmans constant, and T is absolute temperature
[6]. The activation energy, Q, and the stress exponent, n, depend on the creep mechanism, and have
different values at different temperature and applied stress. Equation (1) prescribes a linear relationship in
logarithmic coordinates between the creep strain rate and the applied stress for a specified temperature.
However, the simple power-law model cannot describe the non-linear experimental creep curves over large
stress ranges. A hyperbolic-sine power-law relationship has been proposed and found to predict the
observed behavior at low and high stresses [10,11,12]. At low and medium stresses, the creep strain rate
depends on stress to the power n. At high stresses, the strain rate is an exponential function of stress [3].

Q
n
 = C [sinh ( )] exp

kT

(2)

where C and are materials constants. The steady state creep data for all selected alloy composition at
three aging conditions (as-cast, and 100h and 250h at 125oC) were fitted to equation (2). The fitted creep
model parameters for the alloy compositions are given in Table 3:
Table 3 The Creep Model Parameters for Selected Alloy Compositions at Different Aging
Conditions
Aging
Alloy
Hyperbolic-sine power-law model parameters
conditions
compositions
C

n
Q (J/mole)
Sn-4Ag-1.5Cu
0.48
0.05
5.9
53000
Sn-4Ag-0.5Cu
0.17
0.14
4.2
55000
As-cast
Sn-2Ag-1.5Cu
2.1
0.09
5.6
55000
Sn-2Ag-0.5Cu
0.3
0.19
4.0
66000
Sn-3.5Ag-0.8Cu
1.46
0.09
4.9
60000
Sn-4Ag-1.5Cu
1.6e-3
0.14
4.9
55000
Sn-4Ag-0.5Cu
0.04
0.21
4.4
54000
100h at
Sn-2Ag-1.5Cu
0.014
0.25
4.1
55000
125 oC
Sn-2Ag-0.5Cu
1.42
0.2
4.6
65000
Sn-3.5Ag-0.8Cu
6.54E-4
0.27
4.3
60000
Sn-4Ag-1.5Cu
5.7E-4
0.2
4.2
54000
Sn-4Ag-0.5Cu
5.1E-3
0.25
5.6
55000
250h at
Sn-2Ag-1.5Cu
1.4E-2
0.27
4.3
55000
125 oC
Sn-2Ag-0.5Cu
8
0.2
4.8
66000
Sn-3.5Ag-0.8Cu
8.68E-2
0.22
4.2
60000
Taking the Sn-4Ag-0.5Cu alloy in the as-cast condition as an example; the curve-fitted hyperbolic-sine
creep model is given below:

55000
4.2
D = 0.17[sinh (0.14 )] exp

kT

(3)

Figure 18 shows the calculated data using the above creep model equation. The model agrees with the
experimental data at the different test temperatures. The presented model parameters in Table 3 provide a
description for the selected alloy compositions at different aging conditions. Comparison of the hyperbolicsine creep model data for these selected Sn-Ag-Cu alloys, show that the stress exponent n varies from 4.1

to 5.9, while the activation energy Q varies from 53000 J /mol to 66000 J/mol. The fitted value of
parameters C and varied with alloy composition at different temperature and aging times. The physical
meaning of these parameters needs further investigation.

Figure 18 - Comparison of Mmodel and Experimental Creep Data for Ascast Sn-4Ag-0.5Cu

Conclusions
The mechanical and microstructural properties of Sn-Ag-Cu alloys with Ag varying from 2wt% to 4wt%
and Cu varying from 0.5wt% to 1.5wt% were systematically studied. An advanced specimen preparation
process was developed using rectangular cross-section small glass tubes. The oil quenched specimen
microstructure was comparable to that of a reflow soldered CSP solder joint.
Youngs modulus as a function of alloy composition only ranged from 37-41 GPa as-cast and decreased to
30-32 GPa after aging for 100h and 250h at 125 oC. The distribution of 0.2% strain yield stress and ultimate
tensile strength as a function of alloy composition was more significant. Both are significantly higher for
the high level of silver and copper composition and gradually decreased to the lowest value for low silver
and copper compositions. The absolute value of yield stress and ultimate tensile strength both decreased
during the high temperature aging process.
The tensile creep behavior was investigated at three temperatures (22oC, 100oC 150oC) for five selected
alloy compositions (Sn-4Ag-1.5Cu, Sn-4Sg-0.5Cu, Sn-2Ag-1.5Cu, Sn-2Ag-0.5Cu, Sn-3.5Ag-0.8Cu) ascast, after aging at 125OC for 100 hours and after aging at 125OC for 250 hours. The creep resistance
decreased as the testing temperature increased for all alloy compositions. For each alloy composition, the
creep resistance decreased as the aging time at 125oC increased. Sn4Ag1.5Cu had the highest creep
resistance and Sn3.5Ag0.5Cu ranked second, while the curves for Sn2Ag0.5Cu, Sn4Ag0.5Cu and
Sn2Ag1.5Cu were similar.
A hyperbolic-sine power-law creep constitutive model was developed to provide an acceptable description
for all selected alloy compositions at different aging conditions over wide applied stress ranges.
Comparison of the hyperbolic-sine creep model data for selected Sn-Ag-Cu alloy shows that the stress
exponent n varies from 4.1 to 5.9, while the activation energy Q varies from 53000 J /mol to 66000 J/mol.

Acknowledgements
The author would like to acknowledge the research funding support from NASA Marshall Space Flight
Center.
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