Vacuum 133 (2016) 31e37

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Vacuum
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Microstructure and corrosion resistance of laser cladding and friction

stir processing hybrid modification Al-Si coatings on AZ31B
Fenjun Liu a, *, Yan Ji a, Qingsen Meng b, Zengsheng Li a
a
Yulin University, College of Energy Engineering, Yulin, Shaanxi, 719000, China
b
Taiyuan University of Technology, College of Materials Science and Engineering, Taiyuan, Shanxi, 030024, China

a r t i c l e i n f o a b s t r a c t

Article history: Al-Si coatings were prepared on AZ31B magnesium alloy by laser cladding (LC), friction stir processing
Received 11 May 2016 (FSP) and hybrid technology (LC-FSP). The coating microstructure, composition and corrosion resistance
Received in revised form were investigated using scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), X-
7 August 2016
ray diffraction (XRD) and electrochemical measurement. The results indicated that compact, uniform,
Accepted 18 August 2016
Available online 20 August 2016
crack and porous free coatings, which metallurgically bonded to the AZ31B magnesium alloy substrate,
were achieved compared with LC coatings. The coatings mainly consisted of Mg2Si, Al12Mg17 and AlMg
phases. The coatings contained multiplicate Mg intermetallic compounds exhibited better corrosion
Keywords:
Laser cladding
resistance as compared with the untreated AZ31B. The formation of compact and uniform Mg inter-
Friction stir processing metallic compounds in the coatings remarkably improved corrosion resistance as compared with LC
Al-Si coating coatings.
Microstructure © 2016 Published by Elsevier Ltd.
Corrosion resistance

1. Introduction homogenization of microstructure in the laser cladding (LC) coat-

Magnesium, which is one of the lightest structure materials,
shows high specific strength, non-magnetic, well thermal and
electrical conductivity, excellent vibration and shock adsorption
ability when alloying with aluminium, manganese, zinc, rare
earths, thorium and zirconium, etc [1]. Therefore, magnesium al-
loys have been widely applied to the field of electronics, aerospace
and automobile industries [2].
However, magnesium alloys are highly chemically active and are
liable to internal galvanic and atmospheric corrosion. The relatively
poor corrosion resistance has been a serious impediment against its
wider application due to the lack of formation of self-healing pas-
sive surface film [3,4]. Hence, a key issue with respect to the safe
use of magnesium alloys for practical applications is proposed.
Laser surface modification, as one of the positive protective surface
treatments, has been investigated for improving the corrosion
resistance of magnesium alloys, owing to a number of advantages.
For example, small thermal deformation and heat affected zone due
to the localized heating from the laser beam, thereby do not change
the bulk properties of the material; relative refinement and
* Corresponding author.
E-mail address: lfjxcmg@126.com (F. Liu).
ings improve the mechanical properties; controlled dilution of the
LC coatings and metallurgical bonding interface between the
coatings and substrate could enhance the bonding strength [4e6].
Lei et al. obtained dense, crack and porous free Al-Si coatings on the
surface of AZ91D magnesium alloy with saw-tooth shape and good
metallurgical bond using a 5 kW CW-CO2 laser system at room
temperature [7]. Qian et al. found that the laser-remelted Al-Si
coating exhibited better corrosion resistance than as-received
AZ91D and plasma-sprayed Al-Si coating based on both salt spray
and potentiodynamic polarization test [8]. However, rough surface
formation, crack and porous sometimes existed in the coating with
LC.
Friction stir processing (FSP) is a novel severe plastic deforma-
tion technique based on friction stir welding (FSW) invented by
TWI in UK [9]. Since intense plastic deformation can be introduced
into the base material in single or multiple pass without additional
heating, FSP has been proved to be an effective technique for pro-
ducing uniform structure [10e12], adjusting surface composites
[13,14], and modifying the microstructure of Al-based alloys with
high efficiency [15,16]. Sato et al. [17] and Darras et al. [18] achieved
grain refinement and homogenization of the microstructure using a
single FSP pass compared with the as-received magnesium alloy.
Cavaliere et al. [19] found that AZ91 prepared by FSP showed su-
perplasticity with an elongation of 1050% at 300
C and 104 s1

http://dx.doi.org/10.1016/j.vacuum.2016.08.010
0042-207X/© 2016 Published by Elsevier Ltd.
32 F. Liu et al. / Vacuum 133 (2016) 31e37
due to the fine-grained microstructure. Hybrid surface treatment is
an effective method that can obviously improve the corrosion
resistance by preparation of a protective coating on magnesium
alloy [20,21]. Herein, a single pass of FSP was used to process the LC
Al-Si coatings on AZ31B magnesium alloy. Meanwhile, micro-
structure and phase composition of the coatings were also exam-
ined in order to elucidate the corrosion mechanism.
2. Experimental procedures
2.1. Materials
AZ31B magnesium alloy cut from the rolled sheets with a size of
300 mm  300 mm  10 mm was selected for this research. The
chemical composition of the alloy was given in Table 1. The speci-
mens were prepared for coating by initially polishing using Nos.
1000 silicon carbide waterproof abrasive papers followed by
manual cleaning with acetone, alcohol and deionized water in turn.
Commercial powder of aluminum (Al) and silicon (Si) with purity
and particle sizes about 99.95% and 50 mm, respectively, were used
in the study. Al and Si powders were mixed with Si weight ratio of
15, 30, and 45 wt%. The corresponding coatings prepared with the
mixed powders were labeled as LF1, LF2 and LF3, respectively.
Ethylene glycol was added to the mixed Al-Si powders to prepare
the coating paste, which was then coated on the polished surface of
the AZ31B magnesium alloy with a thickness of about 1 mm. The
coated specimens were aired for about 24 h before LC and FSP.
2.2. Laser processing and friction stir processing
In order to prepare a sufficient width of the LC coating, a 3 kW
semiconductor laser (SISTAN 3000, China) with a wavelength of
976 nm and diameter of 15 mm for beam was used for LC pro-
cessing. The focal point was fixed at the coated surface of speci-
mens, and the scanning power and speed were set to be 2 kW and
280 mm/min, respectively. Meanwhile, high purity argon was used
as shielding gas. All light spots have a 40% overlap with each other.
After laser processing, the LC coatings were then processed by FSP
implemented using a FSW-LM2-3012 friction stir welding equip-
ment with a cylindrical three spiral line groove tool having a
shoulder of 18 mm diameter and no pin. A single pass FSP was
carried out by use of a tool rotation rate of 1500 rpm, a traverse
speed of 100 mm/min, a tool tilt angle of 2.5
, and a plunge depth of
0.2 mm.
2.3. Microanalysis
For microstructure observation in the cross-section of Al-Si
coatings, the specimens were initially sectioned perpendicular to
the processing trace using a wire cutting machine. The sectioned
specimens were then polished with waterproof abrasive papers of
different grits ranging from 400 to 2000 mm in succession, followed
by disk polishing with diamond paste of 1.5 mm and 0.5 mm to
achieve a mirror-finished surface. After that, the polished speci-
mens were then cleaned with acetone, alcohol and deionized water
in turn and etched with an etchant constituting of a 5 vol% nitric
acid solution for approximately 5 s by immersion etching to expose
the microstructure features. The microstructure morphology,
Table 1
Chemical composition of the AZ31B magnesium alloy (wt.%).
Al Mn Zn Ca Si Cu Fe
2.5e3.5 0.2e1.0 0.6e1.4 0.04 0.1 0.01 0.005
bonding interface and element distribution of the specimens were
analysed using the VEGA3 LMU scanning electron microscope
equipped with Oxford energy-dispersive spectrometer (X-Max 20).
Meanwhile, Bruker S8 TIGER X-ray diffractometer was also
employed to investigate the phase composition of the coatings at a
potential of 40 kV and current of 60 mA.
2.4. Corrosion resistance
For electrochemical researches, square specimens with 1 cm in
side length were cut from the coatings and from the as-received
(untreated) AZ31B sheets. The specimens were then cleaned with
acetone, alcohol and deionized water in turn before testing. The
corrosion resistances of the Al-Si coated AZ31B and untreated
AZ31B specimens were assessed from potentiodynamic polariza-
tion and electrochemical impedance spectroscopy tests which were
performed using PS-168a electrochemical corrosion test system in
5 wt% NaCl solution at room temperature. The specimens with an
exposed area of 1 cm2 were immersed into the solution. Each
electrochemical measurement was implemented using a typical
three-electrode cell system with the specimen as the working
electrode, a platinum plate as the auxiliary electrode and an Ag/
AgCl (saturated with KCl) electrode as the reference electrode. All
the potentiodynamic polarization tests were carried out at a
scanning rate of 1 mV/s.
3. Results and discussion
3.1. Microstructure
The surface forming characteristics of LC and LC-FSP Al-Si
coatings on AZ31B magnesium alloy was shown in Fig. 1a and
Fig. 1b respectively. The results showed that the flat and smooth
surface of Al-Si coatings was prepared using LC-FSP compared to LC
coatings.
The LC coating (LF3) with the thickness of about 1.5 mm was
prepared on the AZ31B magnesium alloy. Fig. 2 showed the macro-
morphology of the coating. According to the microstructure and
bonding interface, the coating can be divided into the cladding
layer (coating 2), transition layer (coating 1) and substrate (AZ31B).
It was evident that the interface between both the cladding layer
(Fig. 2d) and substrate (Fig. 2b) exhibited well metallurgical
bonding, and obvious porosities existed in the coating. The EDS
analysis shown in Fig. 3 corresponds to the elements distributions
along the line labeled in Fig. 2a. The Mg, Al and Si elements were
detected in the Al-Si coating, the distribution of Mg showed an
increasing trend from the surface of coating to AZ31B substrate
while that of the elements of Al and Si showed a decreasing trend,
due to the fact that both Al and Si elements concentration in the
cladding layer were much higher than that in the as-received
AZ31B magnesium alloy. However, the element of oxygen was
also found in the LC Al-Si coating that was not expected.
During LC processing, laser beam irradiated the preplaced Al-Si
colloidal coating and photon energy was converted into heat and
propagated toward the interior immediately. When the tempera-
ture of the specimen was higher than the coating material and
substrate melting points, molten pool was formed and part of the
molten substrate came into the coating [4,22]. In the present work,
low melting point of AZ31B magnesium alloy together with the
agitation of the high power laser during LC processing, promoted
abundant molten Mg substrate came into the Al-Si coating. Then
the Al-Si coating was severely diluted by Mg element. However, the
Mg
distribution of Mg element in the coating was heterogeneous due to
the insufficient diffusion and convection of the Mg element in the
Bal.
molten pool. Because of the different contents of Mg element in the
 F. Liu et al. / Vacuum 133 (2016) 31e37 33

Fig. 1. Surface forming features of the coatings prepared by (a) LC, (b) LC-FSP.

Fig. 2. SEM micrographs of the LC coating (a) macrostructure, (b) bonding interface between the substrate and coating 1, (c) microstructure of the coating 1, (d) bonding interface
between the coating 1 and coating 2, (e) microstructure of the coating 2, (f) pore in the coating.

thickness direction of the coating, the microstructure, phase con- was exposed to the atmosphere during cooling stage after LC. So the
stituents and element distribution presented different character- coating surface was slightly oxidized [22]. Meanwhile, the bubble
istics. In addition, the laser and argon gas shared the same exit, both generated in the molten pool during LC processing, which existed
then moving together during the LC processing. The Al-Si coating in the interior of the cladding coating due to the rapid cooling.
34
Fig. 3. Qualitative chemical analyses of LC coating scanning from the substrate to the
coating along the line labeled in Fig. 2a.
The SEM morphology of the cross-section of the LC-FSP Al-Si
coating (LF3) was shown in Fig. 4a. The laser-melted zone extended
Fig. 4. SEM micrographs of the LC-FSP Al-Si coating.
F. Liu et al. / Vacuum 133 (2016) 31e37
up to an average depth of about 1.4 mm, which was a little thinner
than the LC coating of 1.5 mm, while was thicker than the cladding
paste thickness of 1 mm. It was obvious that the coating was fine
without pores and cracks, and interface between the claddings and
the substrate presented well metallurgical bonding. What is more,
the top surface of the Al-Si coating (Fig. 4e) was more compact and
uniform than that of the LC coating (Fig. 2e).
During the FSP processing, the LC Al-Si coating was plastified by
the heat coming from the friction between the pin shoulder and the
LC coating and plastic deformation. The thermoplastic softening
metal flowed around the pin tool induced by shear stress, which
was generated from the friction motion between pin tool and LC Al-
Si coating. Meawhile, inter-spiral groove in the pin tool shoulder
can also make the thermoplastic softening metal flow along the pin
tool from advancing side to retreating side. The velocity gradient
existed in the thickness direction for different temperature distri-
bution in the FSP zone. Therefore, the thermoplastic softening
metal was plastified and mixed sufficiently. Finally, a uniform and
densitified Al-Si coating occurred on the surface of AZ31B magne-
sium alloy by combination of dynamic recrystallization and me-
chanical squeezing. Meanwhile, good metallurgical bonding
interface between the Al-Si coating and the substrate is not
affected, seen in Fig. 4b and Fig. 2b.
 F. Liu et al. / Vacuum 133 (2016) 31e37
3.2. Phases composition
XRD technique was used to ascertain the phases presented
within the as-received AZ31B substrate and Al-Si coatings prepared
by LC-FSP. Fig. 5 showed the as-received AZ31B magnesium alloy
substrate consisted of a-Mg and Al12Mg17 intermetallic compound,
whereas in the top part of Al-Si coating was composed of a-Mg,
Al12Mg17, Si, Mg2Si and AlMg. Comparing the Al-Si coatings and the
AZ31B substrate, two new intermetallic compound (Mg2Si and
AlMg) occurred in the coating. In the top part of the Al-Si coating,
the microstructure was featured with dark dendrites and gray
matrix, as shown in Fig. 2e. The EDS result (in wt.%) of the gray
matrix phase was 54.9 Mg, 43.5Al and 1.6O. The atomicity ratio of Al
to Mg of gray matrix phase was 1.39, which corresponded with the
atomicity ratio of Al12Mg17 (~1.42) and then the gray matrix phase
was identified as Al12Mg17. The EDS analysis result of dark dendrites
phase was 63.6 Mg, 32.9Si and 3.5Al. The atomicity ratio of Mg to Si
of dark dendrites phase is 1.98, which corresponded with the
atomicity ratio of Mg2Si (2) and the dark dendrites phase was
identified as Mg2Si.
As indicated by Mg-Al equilibrium phase diagram [23], the so-
lidification temperature of Mg-Al liquid decreased with increasing
Al content. That is, more Al content in the Mg-Al liquid is near to
Al12Mg17 phase region in the Mg-Al phase diagram and favors to the
formation of Al12Mg17. Therefore, the increase of Al content in the
powder meant more formation of Al12Mg17 in the coating, as shown
in Fig. 5. The new intermetallic compounds were a product of the
eutectic reaction and solid solution precipitation change during the
solidification process of LC. In the subsequent FSP process, as the
processing temperature under the solidus temperature far lower
than the melting point, thermoplastic material was squeezed,
mixed and then recrystallized distinctly when flowed around the
pin tool from advancing side to retreating side. Therefore, the top of
LC Al-Si coating was only refined and densified without forming
new intermetallic compound.
3.3. Corrosion resistance
Corrosion resistance of AZ31B magnesium alloy depends on the
properties of the Al-Si coatings developed by LC and LC-FSP. The
results showed that aluminium in signal-phase Mg-Al alloys was
Fig. 5. XRD spectra of the AZ31B magnesium alloy substrate and the LC-FSP Al-Si
coatings.
35
beneficial to improve the corrosion behaviour in chloride media.
And this behaviour has distinctly disclosed for AZ31B, which per-
formed higher corrosion resistance than commercially pure Mg
[24]. In the present work, the Al-Si coatings prepared on the surface
of AZ31B by LC-FSP with different Si content were soaked in the
5 wt% NaCl solution at room temperature to ascertain the corrosion
resistance. Polarization curves were shown in Fig. 6, and corre-
sponding corrosion potentials were shown in Table 2, respectively.
According to the polarization curves and corrosion potentials, the
corrosion resistance of Al-Si coating prepared on AZ31 by LC-FSP
was significantly improved compared with as-received AZ31B.
The maximum corrosion potential of the LC-FSP specimen was
0.478 V higher than that of the bare AZ31B specimen. The corrosion
resistance improvement of Al-Si coatings can be mainly attributed
to a large number of Al12Mg17 and Mg2Si with continous network
distribution formed in the coatings, which block the corrosion to
the substrate.
When as-received AZ31B magnesium alloy was exposed to the
atmosphere or aqueous solutions, magnesium hydroxide and
hydrogen gas were formed by an electronchemical reaction with
water. The corrosion reaction may be expressed as
Mg2þ þ 2OH / Mg(OH)2 (corrosion product) (1)
Magnesium hydroxide formed on the bare surface, which was
stable for the basic range of pH values [2]. However, this surface
film broke down and AZ31B magnesium alloy appeared unpro-
tected in presence of chloride anions. And a soluble magnesium salt
was produced at the magnesium-solution interface by the
following reaction:
Mg2þ þ 2Cl / MgCl2 þ 2e (corrosion product) (2)
Fig. 6. Potentiodynamic polarization curves for as-received AZ31B and Al-Si coatings
prepared by LC-FSP.
Table 2
Corrosion potential (V(SEC)) of Al-Si coating for different preparation method in 5%
NaCl solution.
Coatings Preparation method V(SEC)
AZ31B 1.563
LF1 LC 1.272
LF1 LC þ FSP 1.085
LF2 LC þ FSP 1.191
LF3 LC þ FSP 1.176
36 F. Liu et al. / Vacuum 133 (2016) 31e37

Fig. 7. The potentiodynamic polarization curves (a) and nyquist plots (b) of the bare AZ31B and Al-Si coatings for immersion time of 1 h in a 5 wt% NaCl aqueous solution.

This soluble magnesium salt destroyed the magnesium hy-
droxide protective film, the exposed magnesium alloy reacted
anew with the electrolyte (self-dissolution) at sites where the
protective film was breached. Song et al. [25] found that the
Al12Mg17 intermetallic compound had higher cathodic reaction
activity than the a-Mg solid solution, however its anodic dissolu-
tion rate was much lower below its pitting potential than that of a-
Mg. At their corrosion potentials, the corrosion current density of
Al12Mg17 was much lower than that of a-Mg. This meant that
Al12Mg17 was very stable in NaCl solution and was inert to corro-
sion. Previous investigations have reported that distribution of the
Al12Mg17 determined the corrosion resistance of the Mg-Al alloys
[25e28]. According to the results, the Al12Mg17 intermetallic
compound played a cathode role and accelerated the corrosion rate
of the a-Mg for a low volume fraction, however, for a large volume
fraction serve as an anodic barrier and the general corrosion rate
decreased. Moreover, according to the Mg-Al phase diagram, the
maximum solubility of Al in a-Mg was 12.4 wt%. In the present
work, The Al contents of the different Al-Si coatings were all higher
than 12.4 wt%, which would favor the formation of Al12Mg17 [29].
Therefore, the presence of relatively large volume fraction Al12Mg17
phase network acted as an effective barrier against process of
corrosion attack.
In addition, the Mg2Si intermetallic compound formed in the Al-
Si coating can also slow down the corrosion rate to some extent.
When the Mg2Si intermetallic compound was exposed to the at-
mosphere or aqueous solutions, magnesium hydroxide and silane
were produced by an electronchemical reaction with water. The
corrosion reaction may be expressed as [30].
Mg2Si þ 4H2O / 2 Mg(OH)2 þ SiH4 (3)
And then, a soluble magnesium salt was produced at the
magnesium-solution interface by the corrosion reaction (2). Thus it

Fig. 8. Scanning electron micrograph of the corroded film on top surface of the as-received AZ31B (a) and Al-Si coatings (LF1) prepared by LC (b), and LC-FSP (c).
 F. Liu et al. / Vacuum 133 (2016) 31e37 37

can be seen that the corrosion rate of magnesium alloy decreased Acknowledgment
by preparing Al-Si coating on AZ31B magnesium alloy. Meanwhile,
Such uniform and dense Al-Si coatings can equalize the potential The authors wish to thank the Science and Technology
diversity distribution on AZ31B magnesium alloy, and effectively Department of Shaanxi Province (2015GY167, 2015JM5228 and
decrease the potential difference, exhibiting high corrosion 2016KTZDGY04-03) and Science and Technology Bureau of Yulin
resistance. (2014cxy-05-1) for the financial support given to this work.
The potentiodynamic polarization curves and nyquist plots ob-
tained for the Al-Si coatings and as-received bare AZ31B in a 5 wt%
NaCl aqueous solution are shown in Fig. 7. The maximum corrosion References
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