ARTICLE IN PRESS

International Journal of Adhesion & Adhesives 27 (2007) 409416

www.elsevier.com/locate/ijadhadh

Wetting behaviour and reactivity of lead free AuInSn and BiInSn

alloys on copper substrates
F. Gneccoa, E. Riccia, S. Amorea,b, D. Giurannoa, G. Borzoneb, G. Zanicchib,
R. Novakovica,
a
National Research Council (CNR)Institute for Energetics and Interphases (IENI), Via De Marini, 616149-Genoa, Italy
DCCI-University of Genoa, Via Dodecaneso, 3116146-Genoa (Italy) and Genoa Research Unit of National Consortium of Materials Science & Technology
(INSTM), Italy

Available online 23 October 2006

Abstract
The main objective of this work is to determine the wetting behaviour of lead-free solders on copper substrates in view of their
applications in electronic industry. The wetting behaviour of XInSn (X Au, Bi) ternary molten alloys in contact with copper has
been studied and compared with the corresponding behaviour of their binary subsystems with a particular attention to the InSn/Cu
system. The contact angle measurements on Cu-plates were performed by using a sessile drop apparatus. The solder/copper interface was
characterised by the SEM-EDS analysis.
r 2006 Elsevier Ltd. All rights reserved.
Keywords: Interfaces; Metals; Contact angles; Lead-free solder alloys

1. Introduction
The solder process is determined by the physico-chemical
properties of the liquid solder/solid substrate system and
by the environmental conditions over which the solder
process is carried out. For this reason, a complete
characterisation of the surface properties (surface tension,
surface segregation) [1] as well as of the wetting behaviour
has to be done. The wetting properties of a solder/substrate
system are usually characterised by the contact angle, y, of
the liquid metal drop formed on the solid substrate.
Another important parameter of a liquid metal/solid
substrate system is the adhesion strength, generally
represented by the work of adhesion, WA [2]. The joint
reliability is related to the wettability of the surfaces to be
joined and subsequently, the ability of the joint to retain its
performance. However, in practice the wettability of ller
alloys is often overlooked or ignored by the producers. The
formation of a thin intermetallic compound layer is
desirable to achieve a good metallurgical bond [35].
Corresponding author. Tel.: +39 010 6475724; fax: +39 010 6475700.

E-mail address: r.novakovic@ge.ieni.cnr.it (R. Novakovic).

0143-7496/$ - see front matter r 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijadhadh.2006.09.008

Soft soldering has been adapted to microchip packing

and high-level system assembly [4]. Up to now, the tinlead
solders have a combination of properties superior to those
attained with any other alloy system, and their unique
physical, mechanical and electrical properties have made
these solders attractive for joining at low temperatures [4].
The PbSn phase diagram shows the existence of a simple
eutectic indicating a tendency towards phase separation.
The melting temperature of the eutectic composition
Pb73.9 at%Sn is 456 K [6]. Due to a shallow eutectic,
small variations in the solder composition change the
liquidus temperature slightly. The interface reactions
between the solder and the substrate (Cu, Ni, Fe) are
dominated by the Sn-component. During soldering, the
PbSn solder alloys react with the substrate to form
intermetallic compounds at the interface. An excessively
thick intermetallic layer can be a source of mechanical
weakness in the soldered joints due to the thermal
expansion coefcient and elastic modulus mismatch as
well as the brittle nature of intermetallic compounds [3,7].
It has been experimentally determined and subsequently
theoretically conrmed that at the interface between Snbased solders (SnPb, SnBi, SnAg) and Cu-substrate the

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two intermetallic compounds, Z-Cu6Sn5 (adjacent to

solder) and e-Cu3Sn (adjacent to Cu), are formed [4,8,9].
Lee et al. [9] calculated the nucleation activation energies of
these two compounds at soldering temperatures. When
compared, the Z-Cu6Sn5 resulted energetically favoured.
Depending on the kinetics of growth for a particular solder
alloy/substrate system as well as on the operative conditions, both intermetallic phases grow in the solid state
during ageing at lower temperatures up to a signicant
thickness (420 mm).
The presence of Pb in the PbSn solders affects neither
the formation of the CuSn intermetallic compounds nor
the solid-state growth kinetics of these intermetallics.
However, it has been established that Pb affects many of
the desired properties in the PbSn solders. Indeed Pb
improves the corrosion resistance by the formation of a
tenacious oxide skin on the Pb-rich phase of the PbSn
eutectic, prevents the tin-pest phenomenon, i.e., the b-Sn
to a-Sn transition upon cooling at T 286 K, and lowers
the surface tension of solders with respect to the pure Sn
increasing consequently the wettability of the substrate
[3,4].
In view of environmental and health concerns, the leadfree solders have only recently become a common subject
for fundamental research. Alternative solder alloys do not
meet completely environmental regulations and requirements for the reliability of corresponding properties. The
candidate alloys involve Sn as the base element, Ag, Bi, Cu
and Zn as the major alloying elements and some minor
additions such as In and Sb [4,814]. In the framework of
the Action COST 531 project some alloys of the BiInSn
and AuInSn systems have been proposed as candidates
for a lead-free solder in modern electronic. There are many
literature data on the thermodynamic properties [16], few
data on the surface properties of the BiInSn system and
its subsystems [17], while on the wetting properties as well
as the joining of both, the BiInSn and AuInSn systems
on Cu-substrate a complete lack of data was observed.
Joining studies have been done for different compositions
and temperatures, so that it is difcult to nd experimental
data obtained under comparable conditions [12,15,18]. In
the present work, the sessile drop method was used to
determine the contact angle of some binary and ternary
liquid alloys of XInSn (X Au, Bi) in contact with Cusubstrate.
2. Experimental
The contact angle measurements were performed on
some binary and ternary systems (Table 1) from the
melting point up to 768 K. The alloy specimens were
prepared by mixing high purity metals (99.9999% Marzgrade) for each nominal composition, pre-melted in a
vitreous carbon crucible under a vacuum of P 102 Pa at
a temperature about 100 K above the melting point. The
nal alloy composition was controlled by the SEM-EDS
analysis. The measurements were performed in a horizontal

Table 1
Selected alloys as candidates for lead-free solders
Alloy composition (at%)

Tl (K)

y0 (1)

Tf (K)

yf (1)

tf (s)

In70Sn
In85Sn
Au55In
Au97In
Au82Sn
Au5In81Sn
Au11In84Sn
Au8In88Sn
Bi52In
Bi80In
Bi5In81Sn
Bi8In88Sn

450
485
768
588
582
538
493
503
383
355
483
430

142
165
162
160
143
128
117
127
160
122
92
66

708
690
852
760
695
645
600
602
623
648
608
608

41
23
50
21
34
33
52
39
51
44
39
30

680
400
640
550
300
600
600
550
550
700
620
600

furnace heated by an 800 kHz high-frequency generator

coupled to a graphite heater and thermal shields. Metallic
drops of about 1.0 g were mechanically cleaned by
scratching, and then chemically rinsed with pure ethanol
in an ultrasonic bath. The sample was introduced at the
centre of the chamber, placed on a high purity copper
(99.9999%) substrate (plate + 10 mm), metallographically mirror polished. Before the test, the furnace was
heated and degassed under vacuum (P 104 Pa), then
pure Argon (ArN60) was introduced. The resulting oxygen
pressure, PO2 , was around an average value 106 Pa. The
temperature, monitored by a K-thermocouple placed just
below the specimen, was kept constant within 72 K.
Resting on a perfectly levelled substrate, the sample was
illuminated by an aligned light source and its image was
captured by a CCD camera connected to a PC. A specic
image analysis software, ASTRAviews [19,20] with fast
automatic acquisition (0.5 s) was applied which allows the
contact angle values to be calculated in real time with an
accuracy of about 1%. Contact angles have been measured
in a temperature range from above the liquidus temperature up to a nal value, dened for each specic system, at
which the isothermal conditions were reached. DSC
measurements have been done on the ternary alloys. A
differential scanning calorimeter designed as a Calvet
calorimeter (DSC 111, Setaram), has been used for the
determination of the solidliquid transition temperatures.
The specimens (about 700 mg) were enclosed in a tightsealed tantalum crucible. The calibration of the apparatus
was performed with measurements of the temperature of
pure metallic In, Sn, Pb and Zn elements. Temperatures
were measured at 70.5 K. The DSC analyses were
performed in continuous heating mode at a rate of 1, 3
and 5 K/min. Generally, a series of different runs in various
temperature ranges were made and, in order to verify
consistency, each run was repeated three times. More
details on the working conditions may be found in [21].
The metallographic examinations of the alloysubstrate
interface were accomplished by optical microscopy, SEM
and EDS.

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The wetting behaviour of ternary molten alloys in

contact with Cu-substrate has been studied together with
the corresponding behaviour of their binary subsystems
with a particular attention to the InSn/Cu system and the
effect of a third component, Au or Bi, on it. Once the
wetting experiments were completed and characteristic
parameters mentioned above (Table 1) were determined,
the samples were cooled for about 600 s, and then prepared
for the microstructural characterisation with the aim to
study the reactivity of the systems investigated. A summary
of the results of the characterisation of each alloy tested is
reported in Table 2.
3.1. InSn system

Fig. 1. Selected alloy compositions (a) the AuInSn system and (b) the
BiInSn system.

3. Results and discussion

The selected binary and ternary compositions of the
XInSn (X Au, Bi) alloys are shown in Fig. 1(a) and
(b), respectively. The alloy compositions, the initial contact
angles (y0), the nal temperatures (Tf), times (tf) and the
contact angles (yf) are reported in Table 1. The liquidus
temperatures (Tl) refer to the corresponding binary phase
diagrams [6] or, in the case of ternary systems, the values
obtained by DSC [21].

In the InSn system, the eutectic is formed at intermediate composition, In48.3 at%Sn at 393 K. Some
information on the In50Sn solder in contact with copper
substrate is reported in [4,10,18]. The effect of solder-bath
temperature on the performance of In50Sn alloy has been
studied by [4] at temperatures well above the alloys
liquidus. Poor wettability was observed at temperatures
close to T 488 K, while at higher temperatures an
improvement was observed. Therefore, according to these
tests an increase in the solder temperature is a rst
promising approach to improve the solderability. According to [10], the InSn solders wet Cu by forming SnInCu
intermetallics. The interfacial microstructure is affected by
the high solubility of Cu in In50Sn liquid alloy and by the
participation of In in the intermetallic layer at the solder/
Cu interface, exhibiting two layers consisted of Cu2(Sn,In)
and Cu2In3Sn intermetallics, with the In-rich Cu2In3Sn
phase on the solder side of the interface.
In this work, two InSn alloys were investigated:
In70Sn: The variations of contact angle and temperature as function of time for the In70Sn are shown in Fig.
2. The initial contact angle (the mean value of the left and
right contact angles which differo4%) is close to 1401 at
T 573 K. y starts to decrease after 2 s, and reaches a
constant value yf 411 at Tf 708 K in 680 s. After
cooling the sample was metallogracally prepared in order
to characterise the interface cross section obtained by the
SEM and EDS analyses. Close to Cu-substrate a thick
interface layer (60 mm) of the Cu7In19Sn composition
was identied (Table 2, Fig. 3). In many points adjacent to
the solder alloy the phase Cu13In31Sn (light grey spots)
was detected. It is interesting to notice that Cu-contents of
these phases are very close to the well known intermetallics,
e-Cu3Sn and Z-Cu6Sn5, respectively, formed in the case of
the eutectic PbSn/Cu-substrate [4,9]. The remaining
composition, identied as In74Sn is close to the initial
alloy composition. The changes in composition can be
attributed to the loss of In due to its volatility, as proved by
the spots of In found on the substrate surface near the
drop.
In85Sn: The initial contact angle was close to 1651 at
T 523 K. The spreading was observed starting from

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Table 2
Summary of the results obtained by SEM-EDS characterization of the microstructure of each alloy tested
Initial composition (at%)

Interface composition (at%)

Layer thickness (mm)

Tf (K)

Bulk-phase compositions (at%)

In70Sn

Cu7In19Sn

60

708

In85Sn
Au55In
Au97In

3
40
40
30
o2
6

690
852
760

Au82Sn
Au5In81Sn

Cu11In12Sn
Cu20In14Au
Cu22In
Cu38In
Cu26Sn2Au
Cu2In22Sn1Au

Cu13In31Sn
In74Sn
Cu21In23Sn
Cu33In45Au
Cu39In1Au

695
645

Au11 In84 Sn

Cu4In20Sn1Au

22

600

Au8In88Sn

Cu51In42Sn8Au

20

602

Bi52In

Cu32In

o1

623

Bi80In
Bi5In81Sn

Cu46In
Cu20Sn

7
5

648
608

Bi8In88Sn

Cu9In38Sn

o1

608

Cu50Sn23Au
Cu4In44Sn15Au (near interface)
Cu3In59Sn12Au
Cu7In39Sn8Au (near interface)
In17Sn33Au
Cu33In41Sn23Au (near interface)
Cu6In42Sn8Au
In48Bi (near interface)
In36Bi
Bi37In
Cu40Sn (near interface)
In2Sn39Bi
Sn6Bi (near interface)
Cu8In38Sn

140

700

680

120

640
80
620
60

Temperature [K]

Contact Angle []

660
100

600

580

40

100

200

300

400

500

600

700

Time [s]

Fig. 2. Variations of contact angle (o) and temperature (D) as function of time for the In70Sn (at%) alloy on pure Cu-substrate.

590 K and y reached a constant value yf 231 at

Tf 690 K after 400 s. The EDS analysis has shown the
presence of a thin layer (3 mm) close to Cu-substrate
containing the Cu11In12Sn phase.
The results obtained show that with an increase of Sn in
the solder the contact angle decreases together with the
thickness of the interface layer between solder and Cusubstrate. Accordingly, the wetting behaviour changed
from a dissolutive wetting, characterised by a thick
interface layer to a macroscopically planar, thin layer
formed of Sn-rich alloys. Indeed, in the case of the
In70Sn, the nal contact angle should be considered as

an apparent one due to the evident high reactivity of this

system. The reactivity decreases strongly with an increase
in Sn-content. The value yf 231 obtained for the alloy
with higher Sn-content can be taken as the real equilibrium
value.
3.2. AuIn and AuSn systems
Reactions and characteristics of AuIn microjoints need
to be investigated in detail to establish the suitability of this
system as candidate material for engineering applications
such as microelectronic packing [22]. In order to avoid

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413

open circuits during reow soldering of all components, a

high melting soldering process is required for the bonding
of integrated circuits (IC). A ip-chip bonding with an
AuSn metallization system has been successfully introduced for the mounting of IC [23]. Binary gold containing
alloys investigated in this work were:
Au55In: The variations of contact angle and temperature as function of time for the Au55SIn are shown in Fig.
4. The initial contact angle is close to 1621 at T 773 K. y
starts to decrease after 1 s, and reaches a constant value
yf 501 at Tf 852 K in 640 s. The analyses of the cross
section of this alloy sample showed the formation close to
Cu-substrate of a thick interface layer (40 mm) of the
Cu20In14Au composition (Table 2, Fig. 5). Cu-content
of this phase is very close to that of the Z-Cu2In

intermetallic compound [6]. The reaction between the

Au55In alloy and Cu-substrate led to an increase in the
total volume of the liquid phase. According to [2] the
observed wetting behaviour can be classied as dissolutive
wetting as observed in the case of In70Sn alloy. So, the
contact angle value of 501 observed (Table 1) at the nal
temperature Tf 852 K can also be considered as an
apparent angle.
Au97In: In this case, the presence of higher In-content
justies a decrease in the nal contact angle value, yf 211
at Tf 760 K. A thick interface composed of two layers of
40 and 30 mm was found by EDS. The composition of these
layers was Cu22In and Cu38In, respectively.

Fig. 3. SEM micrograph of a cross section of the In70.3Sn (at%) alloy

on pure Cu-substrate.

Fig. 5. SEM micrographs of a cross section of the Au54.9In (at%) alloy

on pure Cu-substrate.

160
800
140

760
100
740

Temperature [K]

Contact Angle []

780
120

80
720
60
700
0

100

200

300

400

500

600

700

Time [s]

Fig. 4. Variations of contact angle (o) and temperature (D) as function of time for the Au55In (at%) alloy on pure Cu-substrate.

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Au82Sn: Due to a slight dissolution of Cu, the interface

of this alloy remained macroscopically planar and as a
consequence an equilibrium contact angle value yf 341
was reached at the temperature of 695 K (Table 1). In
addition, close to Cu-substrate a thin interface layer
(o2 mm) of the Cu26Sn2Au composition was identied
(Table 2, Fig. 6). In this layer, Cu-content is slightly
different from that in the e-Cu3Sn intermetallic compound,
formed in the case of the eutectic PbSn/Cu-substrate [4,9].
Adjacent to the solder the Cu50Sn23Au phase was
detected.
3.3. AuInSn system
Three ternary alloys that belong to this system have been
investigated:
Au5In81Sn: The mean value of the contact angle of
this ternary alloy at Tf 645 K is yf 331 (Table 1). As in
the case of the Au82Sn alloy, the interface examined by
SEM seems to be macroscopically planar. Close to Cusubstrate a thin interface layer (o10 mm) of the
Cu2In22Sn1Au composition was identied (Table 2,
Fig. 7). It is interesting to note that, also in this case, the
Cu-content of this phase is close to that of the e-Cu3Sn
intermetallic compound [4,8,9]. In many points near the
interface the Cu4In44Sn15Au, Cu3In59Sn12Au and
Sn2In phases were found.
Au11In84Sn: A constant contact angle value yf 521
reached after 600 s and at the temperature Tf 600 K was
observed (Table 1). The SEM and EDS analyses revealed
an interface layer 22 mm thick of composition
75Cu4In20Sn1Au (Table 2).
Au8In88Sn: For this alloy, a contact angle value
y 391 was reached at Tf 602 K (Table 1) and a layer
20 mm thick of composition Cu51In42Sn8Au was
identied by EDS (Table 2). The reduction of In and Sncontent from Au11In84Sn and Au8In88Sn to

Fig. 7. SEM micrograph of a cross section of the 14.3Au5.2In80.5Sn

(at%) alloy on pure Cu-substrate.

Au5In81Sn leads to a sharp reduction in reactivity

despite an increase in T (from 600 to 645 K). Indeed,
among the three alloys considered, the Au5In81Sn alloy
having the highest Au-content is characterised by the
formation of 34 times thinner interface layer (6 mm) in
respect to the Au11In84Sn and Au8In88Sn alloys.

3.4. BiSn system

In the BiSn system, the constituent phases of the
eutectic are terminal solid solutions, as they are in the
PbSn system. The BiSn solder forms a well-dened
eutectic microstructure at all solidication rates. According
to the literature these solders wet Cu by forming Sncontaining intermetallics that resemble the intermetallics
formed by eutectic PbSn [9]. The microstructure of the
BiSn/Cu interface is similar to that formed at PbSn/Cu
interface. The principal intermetallic compound is the
Cu6Sn5. During ageing in the solid state, the Cu3Sn
intermetallic compound is formed and its growth at the
Cu-interface can be observed [4,10,15].

3.5. BiInSn system

Fig. 6. SEM micrographs of a cross section of the Au81.8Sn (at%) alloy

on pure Cu-substrate.

Two binary and two ternary Bi-containing alloys have

been investigated in this work:
Bi52In: A contact angle yf 511 was reached at
Tf 623 K in 550 s (Table 1). By EDS analysis a very thin
interface layer (o1 mm) with composition of Cu32In close
to the d-Cu7In3 [6] was identied (Fig. 8). No dissolution of
Cu was observed. This can be explained by a tendency of
the BiCu system to phase separation [6]. Two intermetallic
compounds, the BiIn and BiIn2 were identied in the bulk
alloy indicating the same alloy composition before and
after experiment. The presence of some spots of the ZCu2In phase was also detected by EDS analysis (Table 2).

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Fig. 8. SEM micrograph of a cross section of the Bi51.5In (at%) alloy on

pure Cu-substrate.

415

Cu9In38Sn composition was identied by EDS analysis

(Table 2).
Bi-containing alloys in contact with copper substrate
exhibit low reactivity. Generally, the wetting of these alloys
increases and the corresponding contact angle values
decrease with a decrease in Bi, exhibiting the minimum
value, yf 301 in the case of the Bi8In88Sn alloy having
only 4 at%Bi.
The high melting point of lead-free solders with respect
to the traditional PbSn alloys is usually a weak point in
electronic package. The addition of Au to the InSn system
increases the melting point of these binary solders, but
might be useful for some applications at higher temperatures. Gold is widely used in electronic industry as contact
and conductor material. At the interface between AuSn
solders and Cu-containing substrates, the brittle AuSn4
phase can be observed [24]. Indium has a much lower
afnity for Au and dissolves Au at a rate 1314 times
slower than Sn. The addition of In into Sn-based solders
facilitates the AuIn2 formation at the interface and inhibits
the AuSn4 formation. Accordingly, the solubility of Au in
the InSn system can be reduced, and an optimised ternary
composition could give a solder with required characteristics. On the contrary, the addition of Bi to Sn-based
solders can reduce melting temperatures, promotes the
wetting, but according to the present results, only a limited
quantity of Bi (o4 at%) is suggested.

4. Conclusions

Fig. 9. SEM micrograph of a cross section of the 14.3Bi5.2In80.5Sn

(at%) alloy on pure Cu-substrate.

Bi80In: For this In-rich alloy, the mean value of the

equilibrium contact angle reached at Tf 648 K was
yf 441 (Table 1). A thin interface layer of about 7 mm
having the composition Cu46In was identied by EDS
(Table 2).
Bi5In81Sn: The mean value of the contact angle of this
ternary alloy at Tf 608 K is yf 391 (Table 1). At the
interface the Cu4Sn phase with a thickness of about 5 mm
was formed (Table 2, Fig. 9). It is interesting to notice that
close to this phase some spots of the Cu40Sn compound
(similar to Zphase) [8,9] were observed. The same
composition was detected in a few points of the solidied
alloy drop.
Bi8In88Sn: The mean value of the contact angle of this
ternary alloy at Tf 608 K is yf 301 (Table 1). Close to
Cu-substrate, a very thin interface layer of the

The wetting behaviour of a certain number of solder

alloys pertaining to the systems of InSn, AuSn, AuIn,
BiIn, AuInSn, and BiInSn in contact with a Cusubstrate has been analysed. Their wetting behaviour
changed from a dissolutive wetting, characterised by the
formation of a thick interface layer (InSn, AuIn),
through a macroscopically planar, thin layer formation
(InSn, AuSn, AuInSn) to the formation of an
extremely thin interface layer (BiIn, BiInSn) or isolated
spots (BiIn) as in the case of Bi-containing solders.
Among these systems, the InSn solders with high Sncontent exhibit wetting characteristics very similar to those
of the PbSn system. In the case of AuInSn alloys, an
increase in In-content increases the interface layer thickness, as it is also observed in the InSn and AuIn alloys.
On the contrary, the behaviour of BiInSn alloys in
contact with Cu-substrate is opposite with respect to that
of the InSn system. Namely, the higher is the In-content
the thinner the interface layer observed. Accordingly, the
BiInSn system exhibits the same behaviour as the BiIn.
In order to improve their wetting characteristics and
consequently the mechanical properties, it is very important to optimise the composition and the joining process
parameters to avoid an excessive growth of the interface
reaction layer.

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Acknowledgement
This work was performed in the framework of the E.C.
Action COST 531 project: Lead-free solder materials.
The authors would like to thank the National Consortium
of Materials Science and Technology (INSTM) for
nancial support (PRISMA project). The authors would
like to thank Mr. C. Bottino, IENI-CNR, Genoa, for
performing the EDS and SEM analyses.
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