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Influence of ZnO Nano-Particles Addition on Thermal Analysis,

Microstructure Evolution and Tensile Behavior of
Sn-5.0 wt% Sb-0.5 wt% Cu Lead-Free Solder Alloy
A. N. Fouda a,*, E. A. Eid b

6a Physics department, Faculty of Science, Suez-Canal University, 41522 Ismailia, Egypt

7b Basic Science Department, Higher Technological Institute, 44629 10th of Ramadan City Egypt
8E-mails: dr_eid_hti@yahoo.com; alynabieh@yahoo.com9Tel. +20 01227507971
10Abstract
11Sn-5wt%Sb-0.5wt%Cu (plain SSC505) and Sn-5wt%Sb-0.5wt%Cu-0.5wt% ZnO (SSC12ZnO) composite solder alloys have been studied. The variation in thermal behavior,
13microstructure and tensile characteristics associated with mixing of 0.5wt% ZnO nano14metric particles to plain SSC505 solder were investigated. A slight increment in the
15melting temperature [Tm= 0.89 oC] was recorded using differential scanning calorimetry
16(DSC) after addition of ZnO. X-Ray diffraction (XRD) analysis confirmed the existence
17of -Sn, SbSn and Cu6Sn5 intermetallic compounds (IMCs) beside some of ZnO planes in
18SSC-ZnO composite solder. Field emission scanning electronic microscope (FE-SEM)
19investigation of SSC-ZnO composite solder revealed a homogenous uniform distribution,
20size refinement of IMCs and -Sn grains. Addition of ZnO nano-metric particles into the
21plain SSC505 enhanced the yield stress YS by ~12% and improved the ultimate tensile
22strength UTS by ~13%. In addition, adding ZnO nano-metric particles was found to be
23effective for reducing ductility by ~ 43% of the plain solder due to the refinement of -Sn
24grains within SSC-ZnO composite solder.

25Keywords: A. functional alloys; B. elastic properties; C. nano-crystalline structure; C.

26composite solder; D. microstructure
271. Introduction
28Sn based alloys are promising for advance electronics components connections as a lead29free composite solder [1]. Recently, high-temperature solders have been widely used in
30various types of applications like assembling optoelectronic components, automobile
31circuit boards, circuit modules for step soldering, etc. [2]. Eutectic composition of gold32tin (Au-20wt% Sn) is the best solder alloy for most applications in optoelectronic
33packaging, because of its high creep resistance, wettability and good reliability [3, 4].
34Certainly, high soldering temperatures could damage the properties of optical fibers and
35sensitive optoelectronics such as lasers, light emitting devices, photodetectors, or
36waveguide devices [2, 5]. To solve this problem, great effort has been made to develop a
37new generation of solders with low melting point, reasonable cost, high dimension
38stability and supporting solder joints performance with increasing miniaturization and
39more input/output terminals [6]. Sn-5wt% Sb solder is one of great potential alternative
40materials, it has stable microstructure, good mechanical properties, high creep and
41corrosion resistance and good solderability (contact angle of about 43 o) [7, 8]. To enhance
42the performance of Sn-Sb solders, a third or more materials was incorporated as
43secondary phase with Sn-based matrix is one of the conventional approaches [9, 10].
44Micro/nano size metallic, intermetallic and oxide particles are the widest used in the
45reinforcement of composite materials [11]. Nano-size oxide, intermetallic, or ceramic
46particles is used to reinforce the composite solders of Sn-Ag and Sn-Ag-Cu (SAC). Many
47researchers were investigated the effect of adding nanoparticles to solder alloys on the

48thermal, structural, and mechanical characterizations [11-15]. However, the secondary

49phase must be sufficiently fine, bond well, stable, has a higher flow resistance than the
50alloy matrix, un-deformable and resist the fracture of solder joint [16-18].
51

The literature survey revealed that no studies have been reported so far on lead-

52free SSC505 solder joints containing nano-metric ZnO particles. Therefore, the present
53work is devoted for investigating the effect of adding nano-metric ZnO particles on
54thermal, microstructure and tensile behavior of Sn5wt% Sb0.5wt% Cu (SSC505) lead
55free solder for trying to improve its microstructure and mechanical characteristics.
562. Experimental procedure
57Zinc oxide (ZnO) nano-sized particles with an average grain diameter of ~0.5 nm was
58selected as a reinforcement oxide because of its capability to form physical bond
59with metallic matrix [19]. Additionally, the main advantages of nano-sized ZnO
60particles is : (i) density of (5.67 g/cm3) which is nearly close to density of Sn-5wt%Sb
61(7.530 g/cm3), (ii) high hardness [150GPa] when compared to Sn-5.0Sb matrix [57GPa],
62(iii) chemical stability and (iv) low cost when compared to other nanoparticles such as
63TiO2, Y2O3, SiC and ZrO2. Sn-5.0wt%Sb-0.5wt%Cu (plain SSC505) solder alloy was
64prepared by melting elements Sn, Sb and Cu of 99.99 % purity at 600 oC in a vacuum
65furnace at 600oC for 3h. The SSC-ZnO composite solder was prepared by mechanical
66mixing of ZnO nano-sized powder into a part of the prepared conventional SSC505
67solder with subsequent remelting in a vacuum furnace at 300 oC for 2 h, followed by
68casting into a stainless steel mold and cooled down to room temperature. The other part
69of the plain solder was remelted at the same conditions. The two solder alloys in the form
70of rods were cold drawn into a wire of 0.8 mm diameter. A part of each alloy was rolled
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71into a sheet of 0.5 mm thick for microstructure investigations. Specimens with a gauge
72length of 50 mm were pulled for tensile testing. Prior to the tensile testing, all specimens
73were heat treatment at a temperature of 150 oC for 2 hours in electric oven. Then, they
74were cooled slowly to room temperature in order to stabilize the microstructure and
75remove the residual defects which produced during the cold drawn process. The densities
76) of plain and composite solders were determined using Archimedes principle. Polished
77samples taken from various sections of the solidified rods were weighted in air and when
78immersed in distilled water using an electronic balance (A&D HM-202) with an accuracy
79of 0.0001 g.
80

For metallographic observations, as-solidified specimens were prepared initially

81by mounting in cold epoxy. They were neatly polished using 3m and 1m alumina
82powder which suspended in distilled water as a lubricant. Final polishing to near mirror83like surface was achieved using 0.3m diamond paste. The as-polished samples were
84chemically etched in a solution of 80% glycerin, 10% nitric acid and 10% acetic acid for
85a few seconds [8-10 sec]. The surface morphology of the samples were characterized by
86using field emission scanning electron microscopy (FESEM) SU8000 series equipped
87with energy dispersive X-ray analysis EDX. X-ray diffractometry (Philips diffractometer
88(40 kV) with Cu K1 radiation ( = 0.15406 nm) was used for XRD measurements. The
89melting temperature and fusion heating of solders were analyzed using a differential
90scanning calorimetry (DSC) Shimadzu DSC-50. Tensile testing was performed by
91straining each specimen to fracture under a strain rate of 4.710-3 s-1 and testing
92temperature of 27 oC.
93
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943. Results and discussion

953.1 Thermal behavior
96For the soldering process, the melting temperature of solder is a crucial parameter,
97because it is the main factor in deciding the process temperature. The melting points of
98the prepared plain and composite solders were accurately determined by DSC
99thermograms. Fig. 1(a-b) shows the endothermic peak as a function of temperature of the
100prepared solders during the heating rate of 5 oC/min. The melting temperatures of the
101plain and composite solders are 237.38 and 238.27 oC respectively. This result is verified
102with other previous studies on SAC composite solders [4, 20, and 21]. The slight increase
103in melting point of the SSC-ZnO composite solder can attribute to the effect of the nano104sized ZnO particles on the rate of solidification. Such particles may serve as retardation
105sites for the solidification process of the IMCs [22].
106

Additionally, the endothermic peak of DSC curve in Fig. 1 is initiated at solidus

107temperature Ts and ended at liquidus temperature TL that is estimated by using intersection

108point between the horizontal tangent of baseline and the tangent line for each side of
109endothermic peak. The features of endothermic peak of synthesized solder alloys are
110summarized in Table 1. For plain SSC505 and composite solders, there is a significant
111difference between solidus temperatures Ts = 2.11oC) and a negligible difference
112between liquidus temperatures TL = 0.13oC). For any alloy to be worthwhile as a solder
113for electronics industry, it must possess certain specific quantities like melting range or pasty
114range which is an essential parameter to estimate the time required for finishing the soldering
115process. The pasty range of plain and composite solder alloys are 23.88 and 21.90C
116respectively. The results reflect that, the solidus and liquidus temperatures of the synthesized

117solder alloys are lower than Sn-5wt% Sb binary solder alloy. On the other hand, Sn-5wt% Sb
118has the smallest pasty range of 10.0C and a higher melting temperature of 246 oC that
119provides a useful compromise between them. [9, 23]
120

The calculated values of fusion heat of both solder alloys are tabulated in table 1. The

121heat of fusion of plain is higher than composite solder alloy [HSSC505 HSSC-ZnO = 36.56 J/g).
122Indeed, The heat of fusion H) plays an important role in packaging technology. Therefore,
123SSC-ZnO composite solder alloy is considered as a promising solder for saving energy
124and/or the consumed energy for its melting process is lower than Sn-5wt% Sb HSn-5Sb = 140.5 J/g)
125by ~37% [9].
1263.2 Microstructure Evolution
1273.2.1 XRD analysis
128Representative x-ray diffraction of plain solder and composite solder are shown in Fig. 2a-b. The
129diffraction pattern exhibits sharp peaks, which are attributed to the crystalline nature of
130the two samples. The qualitative analysis of the peaks reflects the existence of the body
131center tetragonal of -Sn-rich phase. The diffraction planes (101), (110), (021), and (202)
132at angles of (2 29.3o, 41.9o, 42.3o and 60.5 o) respectively, confirm the existence of
133cubic SbSn IMC. Regarding to Fig. 2b, it consists of the same phases which exist in the
134plain solder (Fig. 2a). On the other hand, the emergence of (101) and (002) peaks at
135angles 32.7 o and 34.3 o of ZnO is an evidence of ZnO nanoparticles dispersion within 136Sn matrix. Moreover, disappearance of some ZnO peaks can be attributed to interfere of
137its peaks with the peaks of -Sn phases. However, the slow speed scan (0.02 deg/s)
138conducted on the plain and composite solders revealed several peaks at angles of (2=

13930.36o, 42.88o, 53.65o, 57.58o, 62.33o and 79.71o) that corresponds to Cu6Sn5 IMC. The
140small peaks of Cu6Sn5 IMC assigned to the low volume fraction of the copper in the
141solder matrix. Fig. 3, shows a comparison between diffraction peaks (200) and (101) of
142-Sn for plain and composite solder. One can observe that, the diffraction lines are
143slightly shifted towards lower angles, indicating a refinement of -Sn grain size with
144addition of ZnO nano-metric particles [24, 25].
145 It is well known that, the broadening of XRD peaks of an alloy is caused not only by the
146

small grain size but also by the lattice micro-deformations of the alloy [15]. The

147 crystallite size d and an approximate upper limit of the lattice strain can be evaluated by
148

149

XRD peaks analysis according to the Williamson-Hall formula [25]:

cos

K
2 sin
d

(1)

150where is the peak width at half the maximum intensity (FWHM) in radian of the main
151peak, is the Bragg angle, K is the Scherrer constant (0.9), is average of lattice strain ,
152and is the X-ray wavelength (Cu = 0.15406 nm). When cos was plotted against sin
153using main peaks of -Sn, a straight line is obtained with the slope of 2 and the intercept
154as (0.9/d). Results of linear fitting of extracting data are summarized in table 2. The
155crystallite size of Sn-based supersaturated solid solution was measured to be 116 and
15699 nm for the plain and composite solders, respectively. From table 2, one observed that
157the average of lattice strain of -Sn phase for SSC-ZnO composite solder was higher
158than plain solder. The lattice strains observed in the solid-solution phases during
159solidification are caused not only by defect formation but also by another factor; this
160strain was originally introduced during sample preparation, particularly in crushing of the

161sample [26]. The peaks in the X-ray diffraction (XRD) patterns for composite solder
162broadened. This broadening was supposed to be due to lattice strain. Moreover lattice
163strain is introduced upon phase transition from coarsen -Sn phase to refinement phase.
164The anisotropic strain in the diffraction peaks has the same orientation as the Burgers
165dislocation vectors [24]. That indicates the strain is accompanied by dislocation density,
166which is closely related to defect formation.
1673. 2. 2 Metallographic Observations
168Results of microstructural characteristics of the plain and composite solders are discussed
169in terms of: (i) grain morphology, size, and homogenous distribution, (ii) the presence,
170distribution and morphology of the second phase particles, and (iii) percentage of
171porosity, cracks and voids. Fig. 4, shows two optical images (OM) with same powers of
172magnification for the as-cast plain and composite solders that solidified at cooling rate of
1732 oC/min. Results revealed the plain solder was composed of larger non-equiaxed grains,
174non-uniform solidification microstructure; the large dark islands are rich-Sn grains with
175grain size in the range of 100-140 m. The bright region between Sn grains actually
176consists of mixture of lamellar phases of Sn matrix phase (dark phase) and the circular
177bright dot phase termed as SnSb IMC. Moreover, the finer rich-Sn grains within
178composite solder reveal near-equiaxed grains with average grain size in the range of 9017950 m approximately homogenous distribution and narrower dendrites are shown in Fig.
1804b. The decrement of average grain size of -Sn phase with addition of 0.5 wt% Zinc
181nano-metric particles can attribute to its pinning action on grain boundaries and by the
182second phases resulting in limited grain growth [18]. In Fig. 4b, the -Sn phase is not

183only composed of pure Sn crystals but rather contain several of tiny intermetallic particles
184that scattered throughout Sn matrix. Furthermore, with higher magnification of field
185emission scanning electronic microscope (FE-SEM), the precipitated particles like as
186platelets or scallop morphology of the Cu6Sn5 IMC are observed in both solders (see Fig 5a-b).
187

The precipitation of IMCs within -Sn matrix is confirmed by utilizing energy

188dispersion X-ray (EDX) analysis, the eutectic areas were found to contain Zn, O, Cu, Sb
189and Sn elements in composite solder. Thus, it can be concluded that the network eutectic
190areas are Cu6Sn5 and SbSn besides the ZnO particles as shown in Figs. 6a-c. Stichometric
191analysis of EDX data implies the existence of Sn, Sb and Cu atoms and termed IMCs
192according to the atomic ratio of each element in compound [see table 3]. An identified
193reduction in size of SbSn, Cu 6Sn5 IMCs was confirmed by FE-SEM images (see Figs. 5a194b). This was assigned to ZnO nanoparticles which incorporated into the solder matrix.
195According to the adsorption theory, increasing the adsorption of elements could decrease
196the surface energy and/or decrease the growth of IMCs size [14]. For the composite
197solder, the micro-size of SbSn and Cu 6Sn5 IMCs are larger than the size of the ZnO nano198metric particles. Therefore, the incorporation of active surface ZnO nano-metric particles
199refines the size of IMCs. Previously, similar behavior has been reported [20, 22].
200

The Curve of EDX analyses of a selected area (+) in Fig. 6b shows that, the

201Cu6Sn5 IMC contain 7.01 at. % of Sb element [see table 3]. The existence of antimony
202atoms inside the Cu6Sn5 grain confirms that tin-antimony intermetallic compound might
203be the nucleating agent acting as a heterogeneous nucleation of Cu6Sn5 grains. The
204proposed mechanism for the effect of Sb on IMC formation can be summarized as
205follows; because Sb has higher affinity to the constituent element of Sn in SnCuSb

206ternary system, it will reduce the activity of Sn at the Sn-Cu interface by forming SnSb
207compound, resulting in a decreased driving force for CuSn IMC formation [27]. SnSb
208particles may be initially formed and finely dispersed in the molten solder, and then some
209of them precipitate and become the heterogeneous nucleation sites of Cu 6Sn5 IMC.
210According to the theory of heterogeneous nucleation, the Cu6Sn5 phase prefers to nucleate
211on the SnSb surface in order to reduce the thermodynamic barrier [28]. The increase in
212nucleation probability of Cu6Sn5 grains consequently lends to the refinement of the
213grains. As a result, the small and uniform grains obtained in the composite solder slow
214down the ripening rate, and the refinement effect is achieved
2153.3 Density measurement
216The results of density measurements were conducted on the solidified plain and
217composite solders. In Table 4, all the density values were very close which is predicted
218because of the slight difference in density between Sn and ZnO. The porosity
219measurement was theoretically calculated [12, 24]. The value of porosity implied that the
220higher percentage of pores exists in the case of SSC-ZnO composite solder.
2213.4 Strengthening effect
222Fig. 7 shows the typical tensile stressstrain curves of plain and composite solders
223stretched with constant strain rate of 7.410 -3 s-1 and performed 27 oC. The stressstrain
224obtained curves exhibited plateau shaped with steady stable flow stress of the two solder
225alloys. It was found to be strongly dependent on alloy composition of the tested material.
226Furthermore, steady state flow of composite solder was higher than plain solder by ~12%.
227This observation can be explained as; during plastic deformation the solder alloy suffers
228from simultaneous work hardening and dynamic recovery [17]. They have contrary

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229influences on the mechanical deformation of the alloy. Hence the steady stable stresses
230seem to be represented equal combination effects for those. Additionally, existence of the
231ZnO nanoparticles must increase dislocation densities because of their restricting effect
232for the motion of dislocations, besides the dispersion hardening mechanism of the IMCs.
233Therefore, during deformation, the movement of generated dislocations becomes mixed
234and tangled. It is then more difficult for other dislocations to glide through the material,
235especially at lower testing temperatures leading to increase the flow stresses [20].
236

The average values of Young modulus E, ultimate tensile strength UTS, yield

237stress YS, fracture stress f and ductility of the synthesized solder alloys were tabulated
238in Table 5. Addition of 0.5 wt% ZnO nanopowders was found to have a significant effect
239on the tensile parameters. Detectable increments in E by 52%, UTS by 11% and in YS by
24013% were recorded. However, the ductility of SSC-ZnO composite solder was less than
241plain solder by 43%. Improvement in the tensile parameters was achieved because of
242presence of ZnO nanopowders as reinforcement agent. The nano-sized particles are
243dispersed uniformly and homogeneously distributed in Sn matrix which provide high
244barrier by impeding grain boundary sliding and dislocation movement. The reinforcement
245nanoparticles play two different roles. They may strengthen the alloy matrix and enhance
246the formation of large dislocation pile-ups at grain boundaries. Simultaneously, the higher
247friction of nanoparticles generates microcracks nucleation at the interface between Sn
248matrix and IMCs which speed up the failure process. [29, 30] So, ductility decreased
249because of a large amount of microporosity throughout grain boundaries and crack
250nucleation sites in the form of hard and brittle ZnO nanopowders [20, 24, 31].

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Eventually, the influence of the nano-metric size particles can be summarized in:

252(i) pinning grain boundaries and thus impeding sliding of the grain boundaries, (ii) the
253increase of dislocation densities and obstacles to restrict the motion of dislocation and
254(iii) the dispersion hardening mechanism of the IMCs and ZnO nanopowders. [30, 32]
2554. Conclusion
256ZnO nano-sized particles were mechanically mixed with the molten of SSC505 at 300 oC
257during the fabrication of SSC-ZnO composite solder. Thermal behavior, microstructure
258and mechanical characteristics were discussed. The melting point of SSC505 solder is
259slightly increased after the addition of ZnO nanoparticles. X-ray diffraction analysis of
260SSC-ZnO confirms the existence of SbSn, Cu6Sn5 IMCs and ZnO. The microstructure
261observations revealed finer IMCs due to active surface area of ZnO nanoparticles that
262supports the strong adsorption effect. According to the tensile measurements, an
263improvement in UTS and YS were established. However, the ductility of SSC-ZnO
264composite solder was decreased. The variation in tensile properties is attributed to ZnO
265pinning effect which obstructed dislocations and migration of grain boundaries.

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351Figure caption
352Fig. 1. DSC curves of (a) SSC505 and (b) SSC-ZnO composite solder alloys.
353Fig. 2. XRD profiles of (a) SSC505 solder and (b) SSC-ZnO composite solder alloys
354Fig. 3. Comparison between diffraction peaks of (200) and (101) of -Sn for plain and
355composite solders.
356Fig.4. Optical images showing the grains of (a) SSC505 solder and (b) SSC-ZnO
357composite solder alloys
358Fig. 5. FE-SEM micrographs showing the grains of (a) SSC505 solder and (b) SSC-ZnO
359composite solder alloys
360Fig. 6. High-magnification FE-SEM micrographs with corresponding EDX of
361 intermetallic compound of (a) SbSn (b) Cu6Sn5 (c) eutectic region in SSC-ZnO
362 composite solder
363Fig. 7. StressStrain curves showing the effect of adding 0.5 wt% ZnO nanoparticles to
364

SSC505 plain solder alloy

365
366

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