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Materials and Design: C. Taltavull, B. Torres, A.J. Lopez, P. Rodrigo, E. Otero, A. Atrens, J. Rams
Materials and Design: C. Taltavull, B. Torres, A.J. Lopez, P. Rodrigo, E. Otero, A. Atrens, J. Rams
a r t i c l e i n f o a b s t r a c t
Article history: A high power diode laser (HPDL) was used to produce laser surface melting (LSM) treatments on the
Received 22 October 2013 surface of the Mg alloy AZ91D. Different treatments with different microstructures were produced by
Accepted 28 December 2013 varying the laser-beam power and laser-scanning speed. Corrosion evaluation, using hydrogen evolution
Available online 3 January 2014
and electrochemical measurements, led to a relationship between microstructure and corrosion. Most
corrosion rates for LSM treated specimens were within the scatter of the as-received AZ91D, whereas
Keywords: some treatments gave higher corrosion rates and some of the samples had corrosion rates lower than
Magnesium
the average of the corrosion rate for AZ91D. There were differences in corroded surface morphology.
Laser processing
Polarization
Nevertheless laser treatments introduced surface discontinuities, which masked the effect of the micro-
Scanning electron microscopy structure. Removing these surface defects decreased the corrosion rate for the laser-treated samples.
Ó 2014 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2013.12.069
0261-3069/Ó 2014 Elsevier Ltd. All rights reserved.
C. Taltavull et al. / Materials and Design 57 (2014) 40–50 41
Fig. 3. (a) Macroscopic view of LSM treated AZ91 at laser beam power 375 W and
laser scanning speed 90 mm s1. (b) Representative SEM micrograph of a cross-
section, showing that the laser treatment had modified only the b-phase. (c) Higher
magnification of (b). The microstructure shown corresponds to the laser treatment
named selective laser surface melting (SLSM).
Fig. 2. SEM micrograph of the as-received Mg alloy AZ91 showing second phase
(b-Mg17Al12) along dendrite boundaries.
3. Results
matrix. Higher magnification of the laser-modified b-phase pre-
3.1. Microstructure and surface characterization sented in Fig. 3c shows an eutectic microstructure based on fine
plates of b-Mg17Al12 (light grey) and a-Mg phase (dark grey). The
Fig. 2 shows that the microstructure of the as-received AZ91D microstructure shown corresponds to the laser treatment named
consisted mainly of the Mg matrix (a-Mg) (dark grey areas) and selective laser surface melting (SLSM) [43,49]. Fig. 4 presents the
the second b-phase (Mg17Al12) (lighter grey areas). EDS mapping results using the laser beam power 488 W and a laser scanning
showed the distribution of the main alloying elements (not speed of 60 mm s1. The surface was homogenous with no rem-
shown). nants of graphite paint and there were some localized voids (Fig.
Figs. 3–5 present the typical appearance of the surface after sur- 4a). The cross-section SEM micrograph (Fig. 4b) indicated that
face modifications by LSM, and the corresponding microstructure the microstructure for this intermediate input energy (Table 1) in
observed by SEM cross-sections at different magnifications. Fig. 3 the modified surface layer consisted of fine plates of b-Mg17Al12
corresponds to LSM using 375 W laser beam power and 90 mm s1 phase (light grey) and an a-Mg matrix (dark grey) distributed
laser scanning speed, the lowest input energy used (Table 1). This randomly along the surface, producing an homogeneous and
LSM produced almost no deformation of the treated surface, continuous modified layer (Fig. 4c). In addition, there was some
although the location of the laser treated surface was clear un-melted a-Mg matrix, indicated by the surrounding lines in
(Fig. 3a). There was no remnant of the graphite paint on the laser Fig. 4b. The treated depth was approximately 300 lm. Fig. 5a
treated surface. The SEM micrograph of the cross-section, shown shows that, for the highest input energy (Table 1), i.e. laser beam
in Fig. 3b, indicated that the low input energy caused only modifi- power 600 W and laser scanning speed of 45 mm s1, there was
cation of the b-Mg17Al12 phase without any change in the a-Mg a large deformation of the surface. The complete removal of the
C. Taltavull et al. / Materials and Design 57 (2014) 40–50 43
Table 1
Data of laser input energies for the different laser treatments.
Specimen Laser beam power (W) Laser scanning speed (mm s1) Laser input energy (J m1)
AZ91D
L-AZ91D-375–90 375 90 4.17 103
L-AZ91D-488–90 488 90 5.42 103
L-AZ91D-600–90 600 90 6.67 103
L-AZ91D-375–60 375 60 6.25 103
L-AZ91D-488–60 488 60 8.13 103
L-AZ91D-600–60 600 60 1.00 102
L-AZ91D-375–45 375 45 8.33 103
L-AZ91D-488–45 488 45 1.08 102
L-AZ91D-600–45 600 45 1.33 102
Fig. 6 presents the specific hydrogen evolution volume for the as-
received AZ91D, and the LSM treated samples, as a function of the
immersion time. For all specimens, the hydrogen volume increased
with immersion time. For the as-received AZ91D, the error bars in-
dicate the data variability, as deduced from the three samples tested.
Fig. 6b (magnification of the squared zone in Fig. 6a) indicates that,
with the exception of the lowest laser power, the hydrogen evolu-
tion rate for short immersion times for all the LSM samples was lar-
ger than that for the as-received AZ91D. Fig. 6a indicates that none of
the LSM samples produced a hydrogen evolution rate lower than
that of the as-received AZ91D, taking into consideration the error
bars for the AZ91D. Furthermore, the highest laser-beam powers
produced LSM had hydrogen evolution rates significantly higher
than of the as-received AZ91D. However, as the immersion time
increased, the differences between the hydrogen volume for the
as-received AZ91D and the LSM treated samples reduced, and only
the LSM samples treated at the highest input energies corroded
faster that the as-received AZ91D. The degradation of the other
LSM samples was within the variability of the degradation of the
as-received AZ91D. Some of these samples had corrosion rates lower
than the average corrosion rate for AZ91D.
Fig. 7 presents contour plots of the average corrosion rate
related to laser beam power and laser scanning speed. The black
colour zone represents the average corrosion rate for the as-
received AZ91D, which was 1.3 ± 0.8 mm y1 averaged over the
Fig. 6. Hydrogen evolution data for AZ91D and LSM specimens immersed for 50
first 24 hours and 2.6 ± 1.4 mm y1 averaged over the first 48
hours in 3.5% NaCl. For the LSM samples, the designation gives the laser power and
hours. scanning speed. (b) Detail view of dashed square in (a). The data for AZ91D are
The corrosion rate after 24 hours (Fig. 7a) indicates a correlation given as the full squares, and the error bars indicate data variability. Most of the
between laser parameters and corrosion rate of the LSM treated LSM samples had corrosion rates higher than or within the scatter of the AZ91D
samples. The corrosion rate increased with increasing laser-beam data. At the longer immersion times, some of the samples had corrosion rates lower
than the average of the corrosion rate for AZ91D.
power and decreasing laser-scanning speed. The lowest corrosion
rates corresponded to (i) the lowest laser-beam power (375 W)
and highest laser-scanning speed (90 mm s1), which correspond speeds. After 48 hour most of the lowest input energies laser treat-
to the lowest input energy and SLSM and (ii) middle laser-beam ments provided corrosion rates similar to those of as-received
power (450 W) and middle laser-scanning speed (60 mm s1). AZ91D, and some conditions provided corrosion rates lower than
The highest corrosion rate corresponded to the highest input those of as-received AZ91D.
energies, i.e. 600 W laser-beam power and 45 mm s1 laser-
scanning speed. 3.3. Polarization curves
Fig. 7b indicates that there was a similar correlation for the cor-
rosion rate averaged over 48 hour. The corrosion rate increased Fig. 8 presents typical polarization curves measured after 1 hour
with high laser-beam power and low laser-scanning speeds, and immersion in 3.5% NaCl solution for the as-received AZ91D and
was lowest for low laser-beam power and high laser-scanning LSM samples. Fig. 8a presents the polarization curves for a
44 C. Taltavull et al. / Materials and Design 57 (2014) 40–50
Fig. 7. Contour maps of average corrosion rate evaluated from hydrogen evolution
data averaged (a) over 24 hours, and (b) 48 hours of immersion in 3.5% NaCl related
to laser-beam power and laser-scanning speed. Note that, at the longer immersion
times, some of the samples had corrosion rates lower than the average of the
corrosion rate for AZ91D.
Table 2
Data of corrosion rates for AZ91D-LSM samples in 3.5% NaCl measured by immersion test and electrochemical test represented in Figs. 6 and 8.
Specimens Laser beam Laser scanning Ecorr (VAg/AgCl) icorrTafel (lA cm2) PiTafel (mm y1) PAH (24 h) (mm y1) PAH (48 h) (mm y1)
power (W) speed (mm s1)
AZ91D 1.518 20.2 ± 7.2 0.46 ± 0.16 1.3 ± 0.8 1.6 ± 1.4
L-AZ91D-375–90 375 90 1.527 12.2 0.28 0.9 1.3
L-AZ91D-488–90 488 90 1.522 108.9 2.49 4.0 4.3
L-AZ91D-600–90 600 90 1.480 379.9 8.68 4.1 2.0
L-AZ91D-375–60 375 60 1.524 54.6 1.25 1.8 0.9
L-AZ91D-488–60 488 60 1.488 161.4 3.69 4.9 2.4
L-AZ91D-600–60 600 60 1.488 621.5 14.20 6.1 5.2
L-AZ91D-375–45 375 45 1.523 95.2 2.18 3.1 1.8
L-AZ91D-488–45 488 45 1.481 260.9 5.96 6.6 6.2
L-AZ91D-600–45 600 45 1.500 569.1 13.00 20.9 17.7
Fig. 11. Macroscopic image of the corroded surface of as-treated AZ91D and
AZ91D-LSM samples after measurement of the polarization curve in 3.5% NaCl,
related to laser-beam power and laser-scanning speed. The cell configuration (Fig.
1) produced circular corroded zones, which were the areas in focus.
Fig. 9. Contour map of corrosion rate calculated using Tafel extrapolation method
from polarization curves at one hour immersion in 3.5% NaCl related to laser-beam presented a slightly lower corrosion rate. The data of Fig. 9 are in
power and laser-scanning speed. broad agreement with those of Fig. 7.
Fig. 10 and Table 2 present a comparison between the corrosion
rate evaluated by the Tafel extrapolation and from the evolved
hydrogen averaged over 24 and 48 hours of immersion. These
quantities should be equal so the dotted line is an aid to the eye
and shows the condition for equality. There was an agreement be-
tween the corrosion rates obtained by the Tafel extrapolation and
the hydrogen evolution methods, although there was significant
data scatter.
Fig. 13. (a) Cross-section backscattered SEM micrograph of the corroded surface of
AZ91D-SLSM sample after 54 hour immersion in 3.5% NaCl; (b) arrowed detail 1 in
(a); (c) arrowed detail 2 in (a).
10 showed that the corrosion rate data were consistent with the
expected linear relation between the corrosion rate evaluated from
the evolved hydrogen after 24 or 48 hours and the corrosion rate
evaluated by Tafel extrapolation of the polarization curves,
although there was significant scatter of the data. The contour
plots of Figs. 7 and 9 had many similarities, particularly for the
medium laser power. This analysis indicated that Tafel extrapola-
tion at short immersion times could be used as an indication of
the long-term corrosion behaviour, and that there were none of
the other issues that can cause Tafel extrapolation to give values
not in agreement with independent measurements [44,48,50].
The nature of the laser treatment applied had a strong influence
in the corrosion rate of the laser treated samples, in agreement
with [17]. In general, the corrosion rate increased with increasing
laser input energy, so that the corrosion rate was maximum for
high laser power and low laser-scanning speed (Fig. 7). An analysis
of the complete set of data for the two tested times, indicated that
the relationship between the laser parameters with the corrosion
Fig. 16. Polarization curves of as-received AZ91D and AZ91-LSM at laser power- rate was similar. However, at 48 hours of immersion time (Fig.
beam 600 W and laser-scanning speed 45 mm s1 measured as treated or ground to
1200 grit, in 3.5% NaCl.
7b) there was a significant area of low corrosion rates (represented
by the black area) at intermediate input energy which was not pre-
sent at 24 hours (Fig. 7a). This indicated that the corrosion rate
of 600 W and laser-scanning speed of 60 mm s1. Fig. 15a indicates tended to somewhat stabilize with longer immersion time. In addi-
pits distributed throughout the surface in the cross-section SEM tion, there were laser treatment conditions (black with white lines
micrograph of the LSM corroded sample. The pits were located pre- in Fig. 7b) where the corrosion rate was significantly lower than
ferentially in the defects (voids). The progression of the pitting the average of the as-received alloy, although the scatter of the
hardly depended on the microstructure achieved by the LSM treat- data was not included in this plot. Nevertheless, the fact that this
ment. Fig. 15b shows a large pit that had progressed through the region existed, indicates that this laser conditions needs to be
surface to a depth of 30 lm. There was an intermediate zone where taken into account.
the pitting had not progressed (indicated by the square in Fig. 15b). The differences on the corrosion behaviour of the laser-treated
Fig. 15c presents this zone at higher magnification. There was a specimens have been caused by two main factors: (i) the changes
continuous network of fine b-Mg17Al12, indicated by the arrows in the microstructure by means of the laser treatment [17,22–24]
in Fig. 15c. Nevertheless, Fig. 15d, (corresponding to a magnifica- and (ii) the modification produced in the surface characteristics,
tion of the dashed square in Fig. 15b) indicates that, in other including composition, roughness [51] or residual stress [52].
LSM zones, the microstructure was composed of isolated fine These are analysed separately in the following.
b-Mg17Al12 phase. Figs. 3c, 4c and 5c presented the typical SEM micrographs of the
three main microstructures obtained by the LSM treatments
[53]. Fig. 3c showed the microstructure modification achieved in
3.6. Influence of other parameters
a SLSM treatment (laser-beam power of 375 W and laser-scanning
speed of 90 mm s1) where only the b-Mg17Al12 phase was
Fig. 16 presents polarization curves of (i) as-received AZ91D, (ii)
modified and the a-Mg matrix was unaltered. The laser-modified
a LSM treatment as treated, and (iii) a LSM treatment ground to
b-phase presented a eutectic microstructure based on fine plates
1200 grit after the laser treatment. A displacement of the curve
of b-Mg17Al12 and a-Mg phase [43,49]. The corrosion behaviour
to the left occurred for the ground LSM sample corresponded to a
of the SLSM treatment was pitting combined with slight homoge-
lower corrosion current density, icorr.
neous dissolution of the laser modified b-phase (Fig. 13). This
Fig. 17 shows the corrosion rate calculated by Tafel extrapola-
corrosion behaviour could be explained as a consequence of: (i) a
tion from the polarisation curves for (i) the LSM samples tested
two-phase microstructure similar to that of the as-received
as-treated, and (ii) after grinding to 1200 grit. Table 3 presents
AZ91D, which promoted the formation of micro-galvanic couples
the numeric data for the corrosion rates measured related to the
between the a-Mg and the laser modified b-phase, causing
surface preparation. At the highest input energy, i.e. laser-beam
inhomogeneous corrosion, and (ii) the eutectic microstructure
power of 600 W and laser-scanning speed of 45 mm s1, there
produced by the laser modified b-phase was composed of fine
was a reduction of up to 97% of the corrosion rate after surface
b-Mg17Al12 phase forming a closed network, which implied a pro-
grinding, whereas there was a reduction of 45% for a middle input
tective barrier against the progression of the corrosion attack [35],
energy, i.e. laser-beam power of 488 W and laser-scanning speed of
so if some defect in the surface initiated corrosion, progression
90 mm s1. In addition, the corrosion rates of some laser-treated
along the laser modified b-phase zone was expected to be delayed.
specimens, i.e. laser beam power of 600 W and laser scanning
In the SLSM treatment, the corrosion rate was slightly lower than
speed of 60 mm s1, were lower than those of the as-received
that for the as-received AZ91D, probably due to the reduction of
AZ91D Mg alloy (Table 3).
the number of pits formed, as a consequence of combination of
pitting corrosion (Fig. 13b) and a homogenous dissolution of laser
4. Discussion modified b-phase (Fig. 13c), which is expected to avoid the
formation of a pit in the adjacent a-Mg matrix.
Fig. 6 showed that the hydrogen evolution data indicated that Fig. 4c presented a cross-section of the LSM treatment achieved
the corrosion rate of the as-received AZ91D and the LSM-treated using medium laser input energy, i.e. laser-beam power of 450 W
specimens was essentially constant with immersion time for short and laser-scanning speed of 60 mm s1, for which there was a low
immersion times. For longer times, corrosion progressed less in the corrosion rate (Fig. 7b). The microstructure consisted of fine plates
laser treated samples than in the as-received AZ91D (Fig. 6a). Fig. of b-Mg17Al12 and a a-Mg matrix distributed in a modified surface,
48 C. Taltavull et al. / Materials and Design 57 (2014) 40–50
Fig. 17. Comparison between the corrosion rates calculated for LSM specimens in as-treated and ground to 1200 grit surface conditions in 3.5% NaCl.
Table 3
Data of corrosion rates of AZ91D-LSM samples in 3.5% NaCl measured in as-treated and ground to 1200 grit surface condition represented in Fig. 17.
Specimen Laser beam power (W) Laser scanning speed Ecorr (VAg/AgCl) icorrTafel (lA cm2) PiTafel (mm y1)
(mm s1)
AZ91D 1.518 20.2 ± 7.2 0.46 ± 0.16
L-AZ91D-600–45– 600 45 1.504 41.4 0.90
1200G
L-AZ91D-375–60– 375 60 1.524 11.5 0.20
1200G
L-AZ91D-488–60– 488 60 1.501 8.7 0.20
1200G
L-AZ91D-600–60– 600 60 1.451 7.3 0.10
1200G
L-AZ91D-488–90– 488 90 1.507 13.0 0.29
1200G
L-AZ91D-600–90– 600 90 1.478 85.5 1.95
1200G
producing an homogeneous and continuous modified layer [53]. very different from that of samples with much better corrosion be-
Moreover, because of the fine nature of the b-Mg17Al12, it can be haviour, so that the strong change in the corrosion behaviour must
considered a continuous network of b-Mg17Al12, which seems to arise from factors associated with the surface morphology such as:
act as an effective barrier to the progression of corrosive attack. (i) the existence of defects in the form of voids as a consequence of
The macroscopic analysis of the corroded surface of this LSM treat- the high laser energies used [54], (ii) increase in the roughness of
ment (Fig. 11) indicated a homogeneous degradation of the surface, the surface which implies a higher surface area exposed to the cor-
which was confirmed by the cross-section SEM micrograph (Fig. rosive medium [51], (iii) incorporation of some carbon from the
14). In addition, there was a thin layer on the corroded surface. graphite paint used in the LSM treatments, and (iv) residual stress
As a consequence, the corrosion progression in this LSM treatment due to the high cooling rates [52].
is expected to start as a homogeneous dissolution of the a-Mg ma- Macroscopic views of LSM treated specimens (Figs. 3a, 4a and
trix enriched with aluminium, forming a thin layer on the treated 5a) revealed that surface roughness, surface voids and incorpora-
surface composed of magnesium-aluminium-oxygen (Fig. 14c and tion of graphite, increased with increasing laser input energy in
d) [24]. In addition, the progression of this corrosion mechanism the LSM treatments. This relationship was in agreement with the
was limited by the existing network of fine b-Mg17Al12, causing corrosion rates obtained by hydrogen evolution (Fig. 7) and elec-
the low corrosion rate. Nevertheless, the thin layer contained some trochemical measurements (Fig. 9), which again indicated that
defects (Fig. 14b) and the network of fine b-Mg17Al12 was not these factors had more influence on the corrosion behaviour of
completely continuous, so its effectiveness as a corrosion barrier the laser-treated specimens than the microstructure modifications
was limited. [51]. In fact, the cross-section analysis of the LSM treatment devel-
For the high input energy LSM treatments, the corrosion rates oped at 600 W and 60 mm s1 (Fig. 15) indicates that the corrosion
obtained from hydrogen evolution (Fig. 7) and polarization curves attack occurred because of voids in the surface of the treated sur-
(Fig. 9), indicated degradation in the corrosion behaviour of the face, which promoted crevice corrosion of the surface caused by
LSM treated samples. The microstructure in these cases were not micro-cells formed between voids (anodic behaviour) and the rest
C. Taltavull et al. / Materials and Design 57 (2014) 40–50 49
of the surface (cathodic behaviour) leading to the formation of pits 4) The LSM treatments caused an increase in the corrosion rate
inside the voids. Moreover, the small size of the voids intensified of the LSM, but after eliminating the top part of the treated
these phenomena. Once the pitting corrosion started, the micro- surface by grinding, the corrosion rate decreased up to 97%.
structure formed by the small isolated b-Mg17Al12 phase in a These results reveal that the effect of surface deformation,
a-Mg matrix (Fig. 5c) seemed to prevent the evolution of the residual stress, incorporation of carbon in the modified layer,
corrosion attack, but pits progressed through small heterogeneities and the production of voids in the surface, had more influ-
in the microstructure of the LSM treatment (Fig. 15b). Then corro- ence on the corrosion of the LSM treated samples than the
sion was controlled by the micro-galvanic couple between the microstructural modifications achieved.
b-Mg17Al12 phase and the a-Mg matrix, as in the as-received 5) After grinding, the corrosion rate of the samples was up to
AZ91D, and by the shape of the network of the b-Mg17Al12 phase 70% lower than those of the untreated AZ91D. This indicates
[1,2,5]. that the modification of the microstructure has a positive
To differentiate the role played by the microstructure and the effect in the corrosion evolution of the LSM samples.
surface defects, some samples were grounded and tested, so that 6) In general, laser treatment of AZ91D is a useful method to
the outer zone of the treated surface was removed. Therefore, the improve the corrosion resistance of the AZ91D alloy.
corrosion behaviour of these samples was only conditioned by its
microstructure. Unfortunately, this approach could not be made
for the SLSM samples, as the treated zone was small. Acknowledgements
There was a strong displacement of the polarization curves of
the LSM treated samples after being ground (Fig. 16). The corrosion Authors wish to thank Ministerio de Economia y Competitivi-
rates evaluated for the different samples (Fig. 17) confirmed this dad (project MAT2012–38407-C03–01) and associated FPI grant,
evolution, with corrosion rates that were in some cases two orders and to the Comunidad de Madrid (project S-0505/MAT/0077) for
of magnitude lower than in the as-treated state. Therefore, most of the funding, and the Australian Research Council Centre of
the corrosion observed in the laser treated samples was due to Excellence Design of Light Alloys for support.
surface defects, so the microstructures developed have a much
better corrosion resistance than the as-received samples [22–26].
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