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Article history:
Received 15 December 2014
Received in revised form
22 February 2015
Accepted 25 February 2015
Available online 5 March 2015
Sn5 wt%Sb0.5 wt%Cu (plain SSC505) and Sn5 wt%Sb0.5 wt%Cu0.5 wt% ZnO (SSC-ZnO) composite
solder alloys have been studied. The variation in thermal behavior, microstructure and tensile
characteristics associated with mixing of 0.5 wt% ZnO nano-metric particles to plain SSC505 solder
were investigated. A slight increment in the melting temperature [Tm 0.89 1C] was recorded using
differential scanning calorimetry (DSC) after addition of ZnO. X-Ray diffraction (XRD) analysis conrmed
the existence of -Sn, SbSn and Cu6Sn5 intermetallic compounds (IMCs) beside some of ZnO planes in
SSC-ZnO composite solder. Field emission scanning electronic microscope (FE-SEM) investigation of SSCZnO composite solder revealed a homogenous uniform distribution, size renement of IMCs and -Sn
grains. Addition of ZnO nano-metric particles into the plain SSC505 enhanced the yield stress YS by
12% and improved the ultimate tensile strength UTS by 13%. In addition, adding ZnO nano-metric
particles was found to be effective for reducing ductility by 43% of the plain solder due to the
renement of -Sn grains within SSC-ZnO composite solder.
& 2015 Elsevier B.V. All rights reserved.
Keywords:
Functional alloys
Elastic properties
Nano-crystalline structure
Composite solder
Microstructure
1. Introduction
Sn based alloys are promising for advance electronics components connections as a lead-free composite solder [1]. Recently,
high-temperature solders have been widely used in various types
of applications like assembling optoelectronic components, automobile circuit boards, circuit modules for step soldering, etc. [2].
Eutectic composition of goldtin (Au20 wt% Sn) is the best solder
alloy for most applications in optoelectronic packaging, because of
its high creep resistance, wettability and good reliability [3,4].
Certainly, high soldering temperatures could damage the properties of optical bers and sensitive optoelectronics such as lasers,
light emitting devices, photodetectors, or waveguide devices [2,5].
To solve this problem, great effort has been made to develop a new
generation of solders with low melting point, reasonable cost, high
dimension stability and supporting solder joints performance with
increasing miniaturization and more input/output terminals [6].
Sn5 wt% Sb solder is one of great potential alternative materials,
it has a stable microstructure, good mechanical properties, high
A.N. Fouda, E.A. Eid / Materials Science & Engineering A 632 (2015) 8287
2. Experimental procedure
Zinc oxide (ZnO) nano-sized particles was selected as a reinforcement oxide because of its capability to form physical bond
with metallic matrix [19]. Additionally, the main advantages of
nano-sized ZnO particles is: (i) density of (5.67 g/cm3) which is
nearly close to density of Sn5 wt%Sb (7.530 g/cm3) (ii) high
hardness [5 GPa], [19] (iii) chemical stability and (iv) low cost
when compared to other nanoparticles such as TiO2, Y2O3, SiC and
ZrO2. Sn5.0 wt%Sb0.5 wt%Cu (plain SSC505) solder alloy was
prepared by melting elements of Sn, Sb and Cu ingots of 99.99%
purity. The process of melting was carried out in air at 600 1C for
3 h. The SSC-ZnO composite solder was synthesized by mixing and
stirring ZnO nano-powder within SSC505 molten alloy. In order to
get a homogeneous composition, the alloy was re-melted three
times to produce rod-like specimen with a diameter of about
10 mm. A stainless steel mold was used for casting, then left to
cool slowly. The two solder alloys in the form of rods were cold
drawn into a wire of 0.8 mm diameter. A part of each alloy was
rolled into a sheet of 0.5 mm thick for microstructure investigations. Specimens with a gauge length of 50 mm were pulled for
tensile testing. Prior to the tensile testing, all specimens were heat
treated at a temperature of 150 1C for 2 h in air. Then, they were
cooled slowly to room temperature in order to stabilize the
microstructure and remove the residual defects which are produced during the cooled drawn process. The densities () of plain
and composite solders were determined using Archimedes principle. Polished samples taken from various sections of the solidied rods were weighted in air and after immersed in distilled
water using an electronic balance (A&D HM-202) with an accuracy
of 70.0001 g.
For metallographic observations, as-solidied specimens were
prepared initially by mounting in cold epoxy. They were neatly
polished using 3 m and 1 m alumina powder which suspended
in distilled water as a lubricant. Final polishing to near mirror-like
surface was achieved using 0.3 m diamond paste. The as-polished
samples were chemically etched in a solution of 80% glycerin, 10%
nitric acid and 10% acetic acid for 10 s. The surface morphology of
the samples were characterized by using eld emission scanning
electron microscopy (FE-SEM) SU8000 series equipped with energy
dispersive X-ray analysis (EDX). X-ray diffractometer (Philips diffractometer (40 kV)) with Cu-K radiation ( 0.15406 nm) was
used for XRD measurements. The melting temperature and heat of
fusion were analyzed using a differential scanning calorimetry
(DSC-Shimadzu DSC-50). Tensile testing was performed by straining
each specimen to fracture under a strain rate of 4.7 10 3 s 1 and
testing temperature of 27 1C.
SSC-ZnO
83
238.27 C
SSC505
237.38 C
100
200
300
400
500
TEMPERATURE (C)
3. Results and discussion
Fig. 1. DSC curves of (a) SSC505 and (b) SSC-ZnO composite solder alloys.
Table 1
Comparison of melting temperatures (Tm), solidus temperature (Ts), liquidus
temperature (TL), pasty range (T) and heat of fusion (H) for various solder alloys.
Material Tm (1C) Ts (1C)
TL (1C)
Sn5Sb
SSC505
SSC-ZnO
249
247.33
247.46
9.0
23.88
21.90
246
237.38
238.27
240
223.45
225.56
141
125.52
88.96
El-Dally [9]
This study
This study
84
A.N. Fouda, E.A. Eid / Materials Science & Engineering A 632 (2015) 8287
INTENSITY (arb.units)
INTENSITY (arb.units)
30
40
50
60
70
80
2 (degree)
Intensity (arb.unt)
Fig. 2. XRD proles of (a) SSC505 solder and (b) SSC-ZnO composite solder alloys.
31
32
2 (degree)
SSC505
SSC-ZnO
Fig. 3. Comparison between diffraction peaks of (200) and (101) of -Sn for plain
and composite solders.
cos
k
2 sin
d
A.N. Fouda, E.A. Eid / Materials Science & Engineering A 632 (2015) 8287
85
Table 2
The average crystallite size (d) and lattice strain () for plain SSC505 solder, SSC-ZnO composite solder and SbSn, Cu6Sn5 IMCs.
-Sn (Matrix)
SbSn (IMC)
10 5
10
10 5
55
Cu6Sn5 (IMC)
10 5
300
10 5
565
10 5
346
10 5
588
Cu 6Sn 5
SbSn
-Sn
-Sn
Cu 6Sn 5
SbSn
Fig. 4. Optical images showing the grains of (a) SSC505 solder and (b) SSC-ZnO
composite solder alloys.
Fig. 6. FE-SEM micrographs showing the grains of (a) SSC505 solder and (b) SSCZnO composite solder alloys.
86
A.N. Fouda, E.A. Eid / Materials Science & Engineering A 632 (2015) 8287
Table 3
Energy dispersive R-Ray (EDX) analysis.
Zone
Composition
Phase identication
Sn
Sb
Cu
Zn
O2
Wt%
At%
Wt%
At%
Wt%
At%
Wt%
At%
At%
Wt%
65.43
72.76
83.59
66.01
61.61
40.53
34.57
3.68
8.75
33.99
7.01
6.61
23.56
2.06
27.37
2.98
3.51
4.94
3.60
13.08
Table 4
Results of density and porosity.
SbSn
Sn
SnSb
Cu6Sn5
Eutectic
Sn
Material
Density (g/cm3)a
Porosity (g/cm3)
Reference
Sn5 wt% Sb
SSC505
SSC-ZnO
7.526 7 0.005
7.553 7 0.006
7.5337 0.006
0.50
0.75 7 0.17
0.87 7 0.20
El-Bahay [23]
This study
This study
Sn Sb
Sb
Sn
SSC-ZnO
SSC505
80
10
Energy (keV)
Sn
Cu6Sn 5
STRESS (MPa)
100
Sn Sb
60
40
20
0
0.00
Room temperature
.
-4 -1
=4.710 s
0.05
0.15
0.20
STRAIN
Sn
B
Fig. 8. Stressstrain curves showing the effect of adding 0.5 wt% ZnO nanoparticles
to SSC505 plain solder alloy.
A
Cu
0.10
Sb Sn
Sn
Cu
Cu
10
Energy (keV)
Sn
Sn
Sb
Sn
O2
Cu
Zn
Cu
Sn
10
Energy (keV)
Fig. 7. High-magnication FE-SEM micrographs with corresponding EDX of intermetallic compound of (a) SbSn (b) Cu6Sn5 (c) eutectic region in SSC-ZnO composite
solder.
A.N. Fouda, E.A. Eid / Materials Science & Engineering A 632 (2015) 8287
Table 5
Tensile results at room temperature and strain rate of 4.7 10 3 s 1.
Material
E (GPa)
UTS (MPa)
YS (MPa)
f (MPa)
f %
Reference
44.5
43.4
60.3
35.50
77.48
86.35
25.70
64.68
73.10
42.59
72.80
22
17.0
9.7
El-daly [9]
This study
This study
87
[1]
[2]
[3]
[4]
[5]
[6]
[7]
[8]
[9]
[10]
[11]
[12]
[13]
[14]
[15]
[16]
[17]
[18]
[19]
[20]
[21]
[22]
[23]
4. Conclusion
ZnO nano-sized particles were mechanically mixed with the
molten of SSC505 at 600 1C during the fabrication of SSC-ZnO
composite solder. Thermal behavior, microstructure and mechanical characteristics were discussed. The melting point of SSC505
solder is slightly increased after the addition of ZnO nanoparticles.
X-ray diffraction analysis of SSC-ZnO conrms the existence of
SbSn, Cu6Sn5 IMCs and ZnO. The microstructure observations
revealed ner IMCs due to active surface area of ZnO nanoparticles
that supports the strong adsorption effect. According to the tensile
[24]
[25]
[26]
[27]
[28]
[29]
[30]
[31]
[32]