J Mater Sci: Mater Electron (2012) 23:484–492
DOI 10.1007/s10854-011-0422-x
The effects of temperature gradient and growth rate
on the microstructure of directionally solidified Sn–3.5Ag
eutectic solder
Mevlüt Şahin • Emin Çadirli
Received: 9 April 2011 / Accepted: 28 May 2011 / Published online: 11 June 2011
Ó Springer Science+Business Media, LLC 2011
Abstract The mechanical properties (microhardness,
tensile strength) of alloys are controlled by their micro-
structure, which depends strongly on temperature gradient
(G) and growth rate (V). Thus, it is important to understand
the relationships among G, V and microstructure (rod
eutectic) of Sn–Ag solders. The Sn–3.5 wt% Ag eutectic
alloy was directionally solidified upward with a constant
growth rate, V (16.5 lm/s) at different temperature gradi-
ents, G (1.43–4.28 K/mm) and with a constant tempera-
ture gradient, G (3.93 K/mm) at different growth rates,
V (8.3–500 lm/s) in a Bridgman–type directional solidifi-
cation furnace. The rod spacings (k) have been measured
from both longitudinal section (parallel to the growth
direction, kL) and transverse section (perpendicular to the
growth direction, kT) of the samples. The undercooling
values (DT) were calculated by using V, k and system
parameters (K1 and K2). It was found that the values of k
(kT, kL) decrease while V and G are increasing. The rela-
tionships between rod spacing and solidification parameters
(G and V) were obtained by linear regression analysis. The
dependences of eutectic spacings k on undercooling (DT)
are also analyzed. k2V, kDT, DTV-0.5 and DTG-0.5 values
were determined by using k, DT, V and G values. The
results obtained in this work are compared with the Jack-
son–Hunt eutectic theory and the similar experimental
works. The experimental k2T V value (159.3 lm3/s) is
slightly lower than the result 174.6 lm3/s calculated from
Jackson–Hunt eutectic theory.
M. Şahin  E. Çadirli (&)
Faculty of Arts and Sciences, Department of Physics,
Niğde University, Niğde, Turkey
e-mail: ecadirli@gmail.com
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1 Introduction
Over the years a number of different schemes have been
proposed for clarifying eutectic microstructures. There are
basically two types of regular microstructures, lamellar or
rod. The lamellar and rod eutectic microstructures consist
of parallel plates of the two phases and rods (sometimes
blades) of one phase contained in a matrix of the second
phase, respectively. This latter type of structure has many
potential applications such as heat–transfer materials,
safety plugs, brazing alloys and lead–free solders.
Solder materials play crucial roles in the reliability of
joint assemblies in electronic packaging. Increasing envi-
ronmental and health concerns over the toxicity of lead
combined with strict legislation to ban the use of lead–
based solders have provided an inevitable driving force for
the development of lead–free solder alloys. Sn–Ag eutectic
alloy has been identified as a lead–free solder candidate to
replace Pb–bearing solders in microelectronic applications
because of its enhanced strength, improved creep and
thermal fatigue characteristics, as compared with other
lead–free solder systems [1–6]. Sn–3.5 wt% Ag solder has
a eutectic point of 494 K and contains a uniform dispersion
of fine Ag3Sn compounds, which greatly enhance its
mechanical strength. Solidification behavior and structural
characteristics of eutectic alloys in many systems continue
to attract interest because of their influence on the physical
properties and performance of materials containing eutectic
constituents.
The first extensive model detecting the eutectic spacing
for lamellar and rod eutectics was proposed by Jackson–
Hunt (J–H) [7]. In this model, the necessary conditions for
the stability of lamellar and rod type eutectics are given to
explain (see Fig. 1). The Jackson and Hunt’s (J–H) clas-
sical model [7] gives the following relationship between
J Mater Sci: Mater Electron (2012) 23:484–492 485

eutectic temperature, Co is the difference between the

G: constant
composition in the b and the a phase, fa and fb are the volume
fractions of a and b phases, respectively. Ci is the Gibss–
Thomson coefficient, D is solute diffusion coefficient for the
melt, ha and hb are the groove angles of a/liquid and b/liquid
phases at the three–phase conjunction point. The physical
parameters for Sn–Ag alloy are given in Appendix.
pffiffiffiffi
ΔT The parameter d for rod eutectic is equal to 2 fa and the
parameter P is defined as [7]:
P ¼ 0:167ðfa fb Þ1:25 0  fa  0:3 ð4Þ
unstable stable unstable
Microstructure plays a very important role on the physical
λe λ m λa λM properties of alloys. The aim of this study is to investigate
λ the dependence of microstructure parameters (kT, kL) on
solidification parameters (G and V), calculate undercooling
Fig. 1 The schematic plot of average undercooling DT versus (DT) and compare the experimental results with the results
eutectic spacing k for a given growth rate V; the stable and unstable
of J–H model and other experimental results.
regions, as predicted by the Jackson–Hunt model [7]

the average undercooling DT, the growth rate V and the 2 Experimental details
lamellar spacing k for an isothermal solidification front as:
DT ¼ K1 Vk þ K2 =k ð1Þ 2.1 Sample preparation and metallographic processing

K1 and K2 are the physical parameters of the system, which In the present work, Sn–3.5 wt% Ag alloy was prepared in a
have the following values, vacuum furnace [8–10] by using tin and silver of purity of
K1 ¼ mPCo =fa fb D ð2Þ 99.99%. After allowing time for the melt to become
X homogeneous, the molten alloy was poured into 10 graphite
K2 ¼ 2md ðCi sin hi =mi fi Þ; i ¼ a; b ð3Þ crucibles (200 mm in length, 4 mm ID and 6.35 mm OD)
i
held in a specially constructed hot filling furnace[8–10]
where m = ma mb/(ma ? mb) in which ma and mb are the at approximately 50 K above the melting point of alloy.
slopes of the liquidus lines of the a and b phases at the The molten metal was then directionally solidified from

Fig. 2 a Block diagram of the

experimental setup, b The
details of the Bridgman–type Argon outlet Sample (Alloy)
1. Water pool inlet
directional solidification furnace 2. Water jacket inlet
3. Water pool outlet
4. Water jacket outlet Solid-liquid interface
5. Argon inlet Flow meter Hot stage
Conducting cable Graphite cylinder
Argon and water flow
Glycerol Outer heater
Bridgman Thermocouples
type
Temperature unidirectional Control thermocouple
Controller solidification
Variac furnace Heat shield
Stable water level
Controller Thermocouple

Argon inlet Cold stage Stainless steel

1 2 3 4 5
sample holder

Thermocouples Water jacket

Argon outputs Steel rod

Heating/ Data Logger

refrigerating Drawing
circulato

Synchronous
Direction control motors
unit
(a) (b)

123
486
Fig. 3 The SEM images of
directionally solidified Sn–Ag
eutectic alloy with different
growth rates at a constant
temperature gradient
(G = 3.93 K/mm)
(a) longitudinal section (b)
transverse section (G = 3.93
K/mm, V = 16.5 lm/s)
(c) longitudinal section
(d) transverse section
(G = 3.93 K/mm,
V = 166.6 lm/s)
bottom to top to ensure that the crucible was completely full.
Each sample was then positioned in a Bridgman–type fur-
nace (see Fig. 2) in a graphite cylinder (300 mm in length
10 mm ID and 40 mm OD). In the experimental technique,
the samples were heated in the range of 50–250 K above the
melting temperature to obtain different temperature gradi-
ents and the samples were then growth by pulling it down-
wards by means of different speeded synchronous motors
after the stabilizing the thermal conditions in the furnace
under an argon atmosphere. After 10–12 cm steady state
growth, the samples were quenched by rapidly pulling it
down into the water reservoir. The melting point of Sn–3.5
wt% Ag alloy is about 494 K. The temperature of water in
the reservoir was kept at 283 K with accuracy of ±0.1 K by
using a digital heating/refrigerating circulating bath (model
9102; Poly Science) to obtain a well quenched solid–liquid
interface in the present work. The sample temperature was
also controlled to accuracy of ±0.1 K using an Eurotherm
2604 type controller. Solidifications of the samples were
carried out with different growth rates (V = 16.5–500 lm/s)
at a constant temperature gradient (G = 3.93 K/mm) and
with different temperature gradients (G = 1.43–4.28 K/
mm) at a constant growth rate (V = 16.5 lm/s).
The quenched samples were removed from the graphite
crucibles and cut into lengths typically 20 mm. The longi-
tudinal and transverse sections of rough ground sample
were then cold mounted with epoxy–resin. The mounted
samples were ground flat with 500, 1000, 2500 grit SiC
paper and polished using 6, 3, 1, 0.25 and 0.05 lm diamond
paste. After finishing the polishing process, the samples was
123
J Mater Sci: Mater Electron (2012) 23:484–492
etched 2–3 s with 90 mL H2O, 10 mL, sulfuric acid, 2 gr
CrO3 acid solution. The SEM images of the growth mor-
phologies of directionally solidified Sn–Ag eutectic alloy
with different growth rates (16.5–166.6 lm/s) at a constant
temperature gradient (3.93 K/mm) are given in Fig. 3.
When the growth rate is 16.5 lm/s, the coarse rod eutectics
are obtained. However, with further increasing growth rate
(166.6 lm/s), the fine rod eutectics are observed.
2.2 Measurement of the temperature gradient, growth
rate and rod spacing
The temperature in the sample was measured with K–type
0.50 mm in diameter insulated two thermocouples which
are fixed within the sample with spacing of 10 mm. Cap-
illary alumina tubes (a 1.2 mm OD 9 0.8 mm ID) were
used to insulate the thermocouples from the melt. The ends
of the thermocouples were connected to the measurement
unit consisting of data–logger and computer. The cooling
rates were recorded with a data–logger via computer during
the growth. When the solid/liquid interface reaches to the
second thermocouple, the temperature difference between
the first and second thermocouples (DT) was read from
data–logger record. The time taken for the solid–liquid
interface the thermocouples separated by known distances
(DX) was read from data–logger record. Thus, the value of
growth rate (V = DX/DT) for each sample was determined
using the measured value of DT and the value of DX. The
G value is determined by dividing DT by DX when solid-
ification front is passing.
J Mater Sci: Mater Electron (2012) 23:484–492 487

The growth rates were calculated with two different method [11]. The triangle is formed by joining the three
methods. In the first method, the values of the growth rate neighbouring rod centres, and the average of the sides of
were calculated from the measurements of the time taken triangle corresponded to ktr. The second method is the area
for the solid–liquid interface to pass the thermocouples counting method [12]. The values of kar were measured on
separated by a known distance. In the second method, the the transverse section of sample. In this method, the
total solidification time and solidification distance were average rod spacings, kar were determined from
measured. The ratios of the distances to the times  
1 A 0:5
(V = DX/DT) were calculated to obtain the growth rates. kar ¼ ð5Þ
M N
The rod spacings (kL) were measured with a linear
intersection method [11] on the longitudinal section. Two where M is the magnification factor, A is the total sample
different methods were used to measure the rod spacings cross sectional area and N is the number of rods on the
on the transverse sections. The first method is the triangle transverse section. kT is the arithmetic average values of ktr
Fig. 4 The chemical
composition analysis of Sn–Ag
eutectic alloy by using SEM–
EDX, gray phase (Sn–rich bSn
phase), white phase (Ag3Sn
intermetallic phase), eutectic
liquid phase (nominal casting
phase)

123
488
and kar. The rod spacings measured on the transverse
section (kT) gave more accurate results than the rod spac-
ings measured on the longitudinal section (kL) [13].
3 Results and discussion
3.1 The microstructure and composition analysis
of phases
The microstructures of samples were characterized from
both transverse and longitudinal sections of samples using
LEO scanning electron microscopy (SEM) equipped with
an energy dispersive X–ray (EDX) spectrometers as well as
a computer controlled image system. The SEM images of
growth morphologies for the directionally solidified Sn–Ag
eutectic alloy were shown in Fig. 3. As can be seen from in
Fig. 3, the microstructure consists of regular intermetallic
Ag3Sn rods in the Sn–rich matrix. The Sn–rich matrix
phase appears gray and Ag3Sn phase appears white. At a
reflow temperature of 523 K, Ag has a solubility of 5.03
wt% in the molten Sn, when slowly solidified, Ag atoms
were exist as Ag3Sn in the Sn matrix [14]. EDX analysis
was performed to determine composition of phases in the
Sn–Ag eutectic sample. The EDX analysis was carried out
at 20 keV using the X–ray lines. According to the EDX
results as shown in Fig. 4 and the solubility of components
in each phases, the white phase is Ag3Sn phase (Sn–16.38
wt% Ag) and the gray phase is the Sn–rich bSn phase (Sn–
0.87 wt% Ag). The composition of casting phase (nominal
composition) was also found to be Sn–3.87 wt% Ag. Also,
this value was confirmed by wavelength dispersive X–ray
fluorescence (WDXRF) spectrometry (PANalytical Axios
advanced model).
3.2 The effect of temperature gradient on rod spacing
One of the purposes of this study was to obtain the rela-
tionships among k, V, G and DT for the directionally
solidified Sn–3.5 wt% Ag eutectic alloy at a constant
16.5 lm/s growth rate and at different temperature gradi-
ents (1.43–4.28 K/mm). The variation of k as a function of
G and the relationships between them determined by linear
regression analysis are given in Fig. 5 and Table 1,
respectively. It can be observed that an increase in the
temperature gradient leads to decrease in the rod spacings
for a given constant growth rate as. When the temperature
gradients of the directional solidified samples were in the
range of 1.43–4.28 K/mm, the k values were found in the
range of 4.25–2.46 lm. The average exponent value (0.51)
of the temperature gradient is very close to average expo-
nent values (0.52) obtained by Çadırlı et al. [13, 15] for
Sn–1.2 wt% Cu binary alloys. The exponent value of the
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J Mater Sci: Mater Electron (2012) 23:484–492
V= 16.5 μm/s (constant) λT - G
5 λL - G
λe - G
Rod spacings, λ (μ m)
4
3
2
1 2 3 4 5
Temperature gradient, G (K/mm)
Fig. 5 Variation of rod spacings with temperature gradient at a
constant growth rate
temperature gradient 0.28 obtained by Kaya et al. [10] for
Sn–8.9 wt% Zn eutectic alloy is lower than the value
obtained from this study. The differences between our
exponent value and other exponent values are mainly caused
by uncertainties in some of the thermo–physical properties
of the used alloys.
3.3 The effect of growth rate on rod spacing
To investigate the effect of the growth rate on rod spacing,
Sn–3.5 wt% Ag alloys were directionally solidified at a
constant temperature gradient (3.93 K/mm) and at different
growth rates (8.3–500 lm/s). The variation of k as a
function of V and the relationships between them are given
in Fig. 6 and Table 1, respectively. When the growth rates
of the directional solidified samples were in the range of
8.3–500 lm/s, the k values were found in the range of
5.47–0.62 lm. The increasing of the growth rate causes the
rod spacing to decrease at a constant temperature gradient.
The average exponent value of the growth rate (0.52) is in
good agreement with 0.50, 0.55, 0.43, 0.52, 0.50, 0.51 and
0.48 values obtained by Bromley et al. [16] for Sn–3.4 wt%
Ag, Garcia et al. [17] for Sn–2 wt% Ag, Shen et al. [6] for
Sn–3.5 wt% Ag, Grugel and Brush [18] for Sn–0.9 wt%
Cu, Çadırlı et al. [13, 15] for Sn–1.2 wt% Cu and Kaya
et al. [10] for Sn–8.9 wt% Zn alloys, respectively. Also,
average exponent value of the growth rate 0.52 is a good
agreement with 0.50 predicted by J–H [7] eutectic theory.
Variations of rod spacing with growth rate in the Sn–Ag
eutectic alloy and comparison of the experimental values
with the values obtained by J–H eutectic theory are given
in Fig. 7. The experimental k2T V value (159.3 lm3/s)
obtained in this study is slightly lower than the result
174.6 lm3/s calculated from J–H eutectic theory [7].
J Mater Sci: Mater Electron (2012) 23:484–492 489

Table 1 The measured

Solidification parameters Microstructure parameters
solidification and microstructure
parameters for directionally a
G (K/mm) V (lm/s) DT (K) kT (lm) kL (lm) ke (lm)
solidified Sn–Ag eutectic alloy
and the relationships among k, 1.43 16.5 0.578 4.25 ± 0.15 4.67 ± 0.14 4.26
G, V and DT 2.07 16.5 0.681 3.56 ± 0.11 4.24 ± 0.13 3.64
3.26 16.5 0.832 3.06 ± 0.09 3.07 ± 0.10 2.98
3.93 16.5 0.903 2.89 ± 0.10 2.86 ± 0.08 2.76
4.28 16.5 0.938 2.46 ± 0.09 2.47 ± 0.10 2.66
3.93 8.3 0.540 5.47 ± 0.39 5.46 ± 0.48 4.60
3.93 16.5 0.762 2.89 ± 0.21 2.86 ± 0.20 3.22
3.93 41.5 1.208 1.67 ± 0.13 2.29 ± 0.16 2.06
3.93 83.1 1.710 1.29 ± 0.11 1.40 ± 0.13 1.46
3.93 166.6 2.422 0.86 ± 0.06 0.86 ± 0.07 1.02
3.93 500 4.196 0.62 ± 0.05 0.66 ± 0.06 0.60
Relationships Constant (k) Correlation coefficient (r)

kT = k1G-0.44 k1 = 0.24 (lm0.56K0.44) r1 = -0.974

-0.57
kL = k2G k2 = 0.12 (lm0.43K0.57) r2 = -0.980
ke = k3G-0.43 k3 = 0.25 (lm0.57K0.43) r3 = -0.999
-0.52 1.52 -0.52
kT = k4V k4 = 13.52 (lm s ) r4 = -0.983
kL = k5V-0.52 k5 = 14.19 (lm1.52s-0.52) r5 = -0.983
ke = k6V-0.50 k6 = 13.06 (lm1.50s-0.50) r6 = -0.999
Relationships

k2V = 159.3 (lm3/s)

DTG-0.44 = 10.39 (lm0.44K0.56)
DTV-0.50 = 0.19 (Klm-0.50s0.50)
keDT = 2.55 (Klm) (constant V)
keDT = 2.50 (Klm) (constant G)
kTDT = 2.34 (Klm) (constant V)
kTDT = 2.24 (Klm) (constant G)
kT: The values of the rod spacing obtained from the transverse section of the samples
a
The values of DT are kL: The values of the rod spacing obtained from the longitudinal section of the samples
calculated from the J–H eutectic
theory ke: The values of the rod spacing calculated from the Jackson–Hunt eutectic theory

10 However, k2T V value obtained in this study is nearly

G= 3.93 K/mm (constant) λT - V same with 160 lm3/s value obtained by Bao et al. [19], and
λL - V
5 close to 156.0 and 164.0 lm3/s obtained by Çadırlı et al.
λe - V
[20] and Ourdjini et al. [21] for Al–Cu eutectic alloys,
Rod spacings, λ (μ m)

3
respectively.
2

3.4 The effect of temperature gradient on the minimum

1 undercooling

0.5
The variations of DT as a function of G and k for constant
V are given in Figs. 8 and 9, respectively. When the tem-
0.3 perature gradients of the directional solidified samples
5 10 20 50 100 200 500 1000
were in the range of 1.43–4.28 K/mm at a constant V, the
Growth rate, V (μm/s)
DT values were found in the range of 0.58–0.94 K. It can
Fig. 6 Variation of rod spacings with growth rate at a constant be seen from Fig. 9 that the undercooling increases 1.5
temperature gradient times while temperature gradient is increasing 3 times at a

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490 J Mater Sci: Mater Electron (2012) 23:484–492

10 constant V. As can be seen from Table 1, the dependence

G= 3.93 K/mm (constant) This work of DT on G and k can be expressed as;
J - H model
DTG0:44 ¼ 10:39 lm0:44 K0:56 ð6Þ
Rod spacings, λ (μ m)

3 ke DT ¼ 2:55 K lm ðconstant VÞ ð7Þ

kT DT ¼ 2:34 K lm ðconstant VÞ ð8Þ

The exponent value of the temperature gradient was

1
obtained 0.44 is slightly lower than the 0.51, 0.53 values
obtained by Çadırlı et al. [13, 15] for Sn–1.2 wt% Cu
binary alloy.

0.3
5 10 50 100 500 1000 3.5 The effect of growth rate on the minimum
Growth rate, V (μm/s) undercooling

Fig. 7 Variation of rod spacings with growth rate in the Sn–Ag

The dependences of DT on V and k for a constant G are given
eutectic alloy and comparison of the experimental values with J–H
eutectic theory in Figs. 10 and 11, respectively. When the growth rates of
the directional solidified samples were in the range of
8.3–500 lm/s at a constant G, the DT values were found in
3.5
V= 16.5 μm/s (constant) G= 1.43 K/mm
the range of 0.54–4.2 K. The increasing of growth rate
3.0 G= 2.07 K/mm causes the undercooling to increase and the rod spacings to
G= 3.26 K/mm decrease. It can be seen from Fig. 11, the undercooling
G= 3.93 K/mm
2.5 increased nearly 8 times while the growth rate increased 60
Undercooling, Δ T (K)

G= 4.28 K/mm
times at a constant G.
2.0
As can be seen from Table 1, the dependence of DT on
1.5 V and k can be expressed as:

1.0
DTV 0:50 ¼ 0:19 ðK lm0:50 s0:50 Þ ð9Þ
ke DT ¼ 2:50 ðK lmÞ ðfor G ¼ 3:93 K=mmÞ ð10Þ
0.5
kT DT ¼ 2:24 ðK lm) ðfor G ¼ 3:93 K=mm) ð11Þ
0.0
0 1 2 3 4 5 6 7 From these results, we can conclude; G and V have strong
Rod spacing, λ ( μm) effect on undercooling. The differences between the exponent
Fig. 8 Calculated undercooling values (DT) versus rod spacing (k)
values obtained from our experimental results and other
for Sn–Ag eutectic alloy at a constant growth rate experimental studies may be due to factors such as, purity,
composition of the alloys and solidification conditions.
30
V= 8.3 μm/s G= 3.93 K/mm (constant)
V= 16.5 μm/s (constant) V= 16.5 μ m/s
1 25
V= 41.5 μm/s
V= 83.1 μm/s
0.9 20 V= 166.6 μm/s
Undercooling, Δ T (K)
Undercooling, Δ T (K)

V= 500 μm/s
0.8 15

0.7 10

5
0.6
0

0.5
1 2 3 4 5 6 0 2 4 6 8
Temperature gradient, G (K/mm) Rod spacing, λ ( μm)

Fig. 9 Variation of the undercooling with the temperature gradient at Fig. 10 Calculated undercooling values (DT) versus rod spacing (k)
a constant growth rate for Sn–Ag eutectic alloy at a constant temperature gradient

123
J Mater Sci: Mater Electron (2012) 23:484–492 491

Appendix
5 G= 3.93 K/mm (constant)

See Appendix Table 2.

3
Undercooling, Δ T (K)

Table 2 The physical parameters used for Sn–Ag eutectic alloy

Symbol Unit Value References
1
TE K 494 [14]
ma K (% wt.)-1 –5.82 [14]
0.5 mb K (% wt.)-1 3.13 [14]
CE wt% 96.5 [14]
0.3 Co wt% 99.92 [14]
3 5 10 30 50 100 300 500 1000
fa – 0.9657 [14]
Growth rate, V ( μm/s)
fb – 0.0343 [14]
Fig. 11 Variation of the undercooling with the growth rate at a Ca K lm 0.0834 [23]
constant temperature gradient Cb K lm 0.0826 [23]
ha ° 3.2 [23]
hb ° 11.7 [23]
4 Conclusions D lm2/s 2070 [24]
K1 K s/lm2 0.0071 Calculated from the
The Sn–3.5wt.% Ag eutectic alloy was directionally physical parameters
solidified with different temperature gradients at a constant K2 J lm 1.24 Calculated from the
physical parameters
growth rate, and with different growth rates at a constant
temperature gradient. The dependence of rod spacing (k)
and undercooling (DT) on solidification parameters (G and
V) were investigated. Some of the conclusions derived
from the present study are as follows:
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