Beruflich Dokumente
Kultur Dokumente
Corrosion Science
journal homepage: www.elsevier.com/locate/corsci
Division of Materials, The University of Queensland, St. Lucia, Brisbane, Qld 4072, Australia
Swiss Federal Laboratories for Materials Science and Technology, EMPA, Dept 136, berlandstrasse 129, CH-8600 Dubendorf, Switzerland
School of Material Science and Engineering, Central South University, Changsha 410083, China
d
CAST Cooperative Research Centre, Materials Engineering, University of Queensland, Brisbane, Qld 4072, Australia
b
c
a r t i c l e
i n f o
Article history:
Received 20 December 2007
Accepted 11 April 2008
Available online 26 April 2008
Keywords:
Magnesium
Microstructure
Weight loss
Microgalvanic corrosion
Hydrogen evolution
a b s t r a c t
The inuence of the microstructure, particularly the morphology of the b-phase, on the corrosion of Mg
alloys has been studied using AZ91 as a model Mg alloy. The corrosion behaviour was characterized for
ve different types of microstructure produced by heat treatment of as-cast AZ91. The inuence of microstructure can be understood from the interaction of the following three factors: (i) the surface lms can
be more or less effective in hindering corrosion and more or less effective in controlling the form of corrosion as uniform corrosion or localised corrosion, (ii) the second phase (the b-phase in AZ91) can cause
micro-galvanic acceleration of corrosion and (iii) the second phase can act as a corrosion barrier and hinder corrosion propagation in the matrix, if the second phase is in the form of a continuous network. It is
expected that these factors are important for all multi-phase Mg alloys because all known second phases
have corrosion potentials more positive than that of the a-phase. A particular example of the corrosion
barrier effect is provided by the ne (a + b) lamellar micro-constituent; when a b-phase plate nucleates
this micro-constituent, the b-phase plate acts as a corrosion barrier. In contrast, nano-sized b precipitates,
produced by aging, caused micro-galvanic corrosion acceleration of the adjacent a-phase. However, it is
an important nding that the corrosion rate of the a-phase was decreased by the aging treatments that
caused the precipitation of the nano-sized b particles.
2008 Elsevier Ltd. All rights reserved.
1. Introduction
Mg alloys are of signicant interest to the automobile and aerospace industries due to their low densities and adequate strength/
weight ratios [13]. A signicant limitation, however, is their corrosion performance [411]. It is important to understand the factors that inuence their corrosion and to understand the
conditions necessary to achieve adequate corrosion performance.
Their corrosion behaviour has been investigated [1222] over the
past decade in order to facilitate their use in structural applications. Mg alloys are often multi-phase and their corrosion performance is inuenced by their microstructure, in particular the
amount and distribution of the different phases.
AZ91 is one of the most popular of the cast magnesium alloys,
with nominal composition Mg9 wt% Al1 wt% Zn. The AZ91 ascast microstructure has typically a primary a-phase matrix and
a divorced eutectic distributed along the a-phase grain boundaries
[6,14,16,2327]. The divorced eutectic typically consists of large bphase particles and the eutectic a-phase. The eutectic a-phase is
super-saturated with Al and can transform, by discontinuous precipitation of the b-phase during cooling from the eutectic temperature, to form a ne lamellar arrangement of a + b [2427]. There
have been several studies [14,16,21,28] of the role of microstructure on the corrosion of AZ91. The corrosion behaviour of the
a-phase and the b-phase are the foundations on which to build
an understanding of the inuence of the microstructure of multi-phase alloys like AZ91. Song et al [13,14] have shown that the
free corrosion potential of the b-phase (1.3 V) is 0.3 V more
positive than the free corrosion potential of the a-phase
(1.6 V) in sodium chloride solutions. The a-phase corrodes
due to its very negative free corrosion potential and there is the
tendency for the corrosion rate of the a-phase to be accelerated
by micro-galvanic coupling between the a-phase and the b-phase.
The b-phase, in contrast, has a relatively lower corrosion rate, is a
more efcient site for the cathodic reaction and may act as a barrier against corrosion propagation [6,13,14,29]. Thus, the b-phase
has two different inuences on the corrosion behaviour: the bphase can act as a galvanic cathode to accelerate corrosion and
the b-phase can act as a corrosion barrier to hinder corrosion.
The micro-galvanic corrosion acceleration is dependent on the anode (a)/cathode (b) area ratio whereas the b-phase acts to hinder
corrosion if it is nely divided and continuous. The corrosion
behaviour of AZ91 can be changed by changes in the amount
1940
2. Experimental procedure
2.1. Materials
The AZ91D
0.14 wt% Mn,
<0.002 wt% Cu
Mg had the
0.008 wt% Mn,
These two Mg alloys are high purity because they both contain
low levels of the impurity elements Fe, Ni and Cu, so the results
of the present research should be directly comparable with the
prior studies [5,6,1316].
The AZ91 specimens were cut from an as-cast ingot and were
subjected to heat treatment as follows. Homogenization annealing
(HA) heat treatments of as-cast specimens were carried out at
380 C and 410 C for 125 h followed in each case by air cooling
(AC); the resulting specimens are designed as HA3805, HA3810,
HA4105, HA4110 and HA4125, where the rst two numbers indicate the temperature of the HA heat treatment (380 C and
410 C) and the second two numbers designate the time in hours
of the HA heat treatment. The solid solution (SS) heat treatment
consisted of heat-treating as-cast specimens at 410 C for 100 h
followed by water quenching (WQ), designed as 4100S (or SS condition). Solid solution treatment plus ageing (SA) consisted of the
solid solution heat treatment followed by an ageing heat treatment
at 200 C for 5, 10, 24 and 48 h; the full designation was
4100S205A, 4100S210A, 4100S224A and 4100S248A, respectively;
the short designation was SA205, SA210, SA224 and SA248. HA and
aging was carried out to produce 4125HA225A (HA for 25 h at
410 C, AC, aging for 25 h at 200 C), 3801S205A (HA for 1 h at
380 C, WC, aging for 5 h at 200 C) and 3810S205A (HA for 10 h
at 380 C, WC, aging for 5 h at 200 C).
The microstructure was examined by optical microscopy and
scanning electron microscopy (SEM) after metallographic preparation by mechanical grinding successively to 1200 grit SiC paper,
polishing successively to 0.5 lm diamond, washing with distilled
water, drying with warm owing air and etching in 3% nital.
X-ray diffraction (XRD) using CuKa radiation was used to characterize the phases present in these samples.
2.2. Corrosion evaluation
The corrosion behaviour was evaluated using separate immersion tests of duration of either 48 h or 96 h, at room temperature,
in 1 N NaCl aqueous solution, which was made with analytical
grade reagent and distilled water. The corrosion rate was evaluated
by measuring (i) the evolved hydrogen during corrosion in the 1 N
NaCl solution and (ii) the weight lost by the specimen. The AZ91
specimens were encapsulated in epoxy resin so that a surface, with
dimension 18 mm 27 mm, was exposed to the solution. The
working surface was mechanically ground to 1200 grit SiC paper,
washed with distilled water, dried with warm owing air, dried
in a desiccator for 1 to 2 days and weighed, to give the specimen
weight before exposure, Wb. The specimen was horizontally immersed in 1500 ml of test solution and the hydrogen evolved during the corrosion experiment was collected in a burette above the
corroding sample. The evolved hydrogen is a direct measure of the
corrosion rate [46,3233], as, in the overall magnesium corrosion
reaction
Mg + H + H2 O = Mg2 + OH + H2
showed that there was negligible weight change of the encapsulating epoxy resin by similar exposures to the 1 N NaCl solution or to
the acid cleaning solution. The hydrogen evolution rate can be related to the weight loss rate, and the weight loss rate can be related
to the corrosion rate, using the following conversions [5,6,20,34
36]:
2
2
1941
has the same outline as the eutectic a-phase and is the result of the
discontinuous precipitation of the b-phase. These ne lamellar
(a+b) micro-constituents and associated large b particles were
interconnected and formed an interconnected network throughout
the microstructure. In addition, the remainder of the microstructure contained large eutectic b-phase particles surrounded by the
ne lamellar (a + b) micro-constituent as isolated entities in the
a-phase matrix.
The microstructure provides clues to the mechanism of formation of the ne lamellar (a + b) micro-constituent in the as-cast
AZ91 microstructure. The ne lamellar (a + b) micro-constituent
had a morphology similar to the typical lamellar pearlite colony
in steel and hence the formation mechanism may be similar [37
39]. There were the cases where it appeared that there was a b
plate at the edge of the ne lamellar (a + b) micro-constituent
and it appeared that this b plate had nucleated the ne lamellar
(a + b) micro-constituent in a mechanism that was similar to the
nucleation of lamellar pearlite in steels as illustrated in Fig. 2
[3739]. The formation of the ne lamellar (a + b) micro-constituent occurs after solidication is complete and it occurs by a solidstate transformation of an a-Mg phase super-saturated in Al. During the transformation, Al is rejected from the a-Mg. If the Al diffusion is not sufciently fast, Al accumulates at the interface and
a b-plate forms when the Al content reaches a critical value. Therefore, the rejection of Al from the super-saturated a-Mg in the ascast AZ91 can lead to the formation of an interface b plate that
can nucleate the ne lamellar (a + b) micro-constituent. After
nucleation, the ne lamellar (a + b) micro-constituent grows due
to the slow diffusion of Al in the Al-rich matrix. This proposed formation mechanism for the ne lamellar (a + b) micro-constituent
is also consistent with instances [16] where the ne lamellar
(a + b) micro-constituent forms when die-cast AZ91 is aged at a
low temperature, e.g. 200 C. In Mg die-casting, molten metal is
rapidly injected into a steel die, solidication is relatively rapid
and the formation of the ne lamellar (a+b) micro-constituent is
prevented. During ageing of die-cast AZ91 at a low temperature,
the ne lamellar (a + b) micro-constituent nucleates from large b
particles. Therefore, it is reasonable that the ne lamellar (a + b)
micro-constituent nucleates from a large b particle and grows
away from the b particle as shown in Fig. 2 for the nucleation
and growth of pearlite in steels. Fig. 2 presents the mechanism of
transformation of austentite (c) to pearlite (the eutectoid microconstituent containing ferrite (a) and cementite in a lamellar
arrangement). The pearlite is nucleated by a cementite plate at
the nucleating grain boundary [3739].
1942
homogenization annealing temperature and/or a longer time produced a more homogeneous distribution of the b-phase throughout the microstructure.
3.3. Microstructure-solid solution (SS)
The microstructure in the solid solution (SS) condition was
homogenous, largely single a-phase and the b-phase was almost
completely dissolved as illustrated in Fig. 4a.
3.4. Microstructure-solution heat treated and aged (SA)
Fig. 2. Pearlite nucleation at a cementite plate during the transformation of austenite (c) to ferrite (a) in steel. Pearlite is a lamellar arrangement of cementite
(carbide, Fe3C, grey) and ferrite (a, white). As the austenite (c) transforms to ferrite
(a), carbon is rejected from the ferrite and consequently the carbon concentration
builds up at the a/c interface until a carbide forms at the interface. Subsequently
pearlite grows from this carbide [3739].
The solid solution and aged microstructures, Fig. 4be, consisted of the a-Mg matrix with numerous nano-sized b precipitates, which were different in morphology to the b-phase
particles in the as-cast and the HA conditions. The b precipitates
in the solution treated and aged (SA) conditions where needle like,
had an average size of 100 nm in width and had a relatively
homogenous distribution throughout the microstructure. Furthermore, the volume fraction of b precipitates increased noticeably
during aging and their size grew somewhat with an increase of
the ageing time as shown in Fig. 4be. Nevertheless, all the b precipitates where needle like with most of the needles oriented in the
same direction in each grain examined.
3.5. Microstructure-homogenization anneal and aged (SA)
The 4125HA225A microstructure (Fig. 4f, HA for 25 h at 410 C,
AC, aging for 25 h at 200 C) was somewhat similar to SA224
(Fig. 4d). The 4125HA225 microstructure consisted of the a-Mg
matrix with numerous needle-shaped b precipitates, size of
100 nm in width, but in 4125HA225 the needles were oriented
in a number of distinct directions compared with SA224 wherein
the needles were largely oriented in the same direction.
For the 3801S205A microstructure, Fig. 4g, the HA for 1 h at
380 C did not cause a large change to the as-cast microstructure;
the microstructure contained large eutectic b particles and the ne
lamellar (a + b) micro-constituent similar to the as-cast structure.
There were, in addition, numerous needle-shaped b precipitates,
size of 100 nm in width, with an appearance of being oriented
in a number of distinct directions. These were precipitated from
the super-saturated a-phase solid solution during the aging treatment (5 h at 200 C).
For the 3810S205A microstructure, Fig. 4h, it would be expected
that the HA for 10 h at 380 C would have dissolved most of the
ne lamellar (a + b) micro-constituent and would have dissolved
some of the large b particles; however the microstructure, Fig. 4h
did consist of the a-Mg matrix, large b particles and a signicant
amount of the ne lamellar (a + b) micro-constituent; the ne
lamellar (a + b) micro-constituent might have reformed during
the air cooling from the HA treatment temperature or during
the aging treatment. In addition, there were, numerous ne interconnected b precipitates, size of 100 nm in width, with some
appearance of being oriented. These were precipitated from the
super-saturated a-phase solid solution during the aging treatment
(5 h at 200 C).
3.6. XRD
The XRD spectra of specimens in the as-cast condition, representative HA conditions and a representative SA condition, Fig. 5,
indicated that the second b-phase particles were Mg17Al12 because
all of peaks in the XRD spectra corresponded to either Mg or
Mg17Al12, although the second b-phase was reported to sometimes
be present as Mg4Al3 [4041]. This indicates that AZ91 had a matrix of a-Mg grains with the second b-phase consisting of the inter-
1943
metallic Mg17Al12 for the as-cast condition and for the various heat
treatments.
Fig. 5 also indicates that the relative peak heights for the peaks
associated with a-Mg were different for the different heat treated
conditions. The largest difference was that between the XRD spectrum for the as-cast condition and the other spectra. This difference is associated with the changes in the microstructure. In the
as-cast condition, there was three forms of a-Mg: (i) primary a,
(ii) eutectic a-phase and (iii) a-phase in the ne a + b lamellar
arrangement. In contrast, after heat treatment, there was largely
only the primary a-phase left, as the other micro-constituents
had dissolved during the heat treatment.
1944
1945
2000
HA3810
Intensity
Intensity
as-cast
0
2000
20
30
40
50
60
70
80
0
90 2000
Two-Theta
20
30
40
4100S248A
60
70
80
90
70
80
90
Intensity
Intensity
HA4110
50
Two-Theta
0
20
30
40
50
60
70
80
90
20
30
Two-Theta
40
50
60
Two-Theta
Fig. 5. XRD patterns of specimens in the as-cast condition, representative HA conditions and a representative SA condition. The peaks marked with a diamond are from
Mg17Al12, all other peaks are from a-Mg.
series: the solid solution condition > SA for 48 h at 200 C > SA for
24 h at 200 C > SA for 10 h at 200 C > SA for 5 h at 200 C > pure
Mg. However, there an exception for the solid solution condition:
(i) the hydrogen evolution volume of the solid solution condition
was a little lower than the as-cast condition until about 60 h
immersion and thereafter there was a reverse tendency, and (ii)
the hydrogen evolution volume of the solid solution condition
was a little lower than the SA for 48 h at 200 C until about 80 h
immersion and thereafter there is a reverse tendency.
3.8. Weight loss data
Fig. 7 presents weight loss measurements. Fig. 7a presents the
weight loss data for 48 h immersion and Fig. 7b presents the data
for 96 h immersion. The corrosion rates were signicantly higher
in the 96 h immersions; this is consistent with the accelerating
corrosion rate as shown in Fig. 6. Furthermore, the trends revealed
in the hydrogen evolution data of Fig. 6 are reproduced in the
weight loss measurements presented in Fig. 7.
It appeared that the ne lamellar a + b micro-constituent in ascast AZ91 was somewhat benecial to corrosion. This is proposed
because the as-cast AZ91, with a microstructure containing the ne
lamellar a + b micro-constituent, had a lower hydrogen evolution
rate than all the HA conditions without the lamellar a + b microconstituent in the microstructure, Figs. 6 and 7. Also the HA3805
condition (HA for 5 h at 380 C) had a lower hydrogen evolution
rate than the HA3810 condition (HA for 10 h at 380 C); for these
two conditions, the only microstructure difference was that
HA3805 condition had a small amount of the ne lamellar (a + b)
1946
Group A
10
8
6
4
2
60
50
40
30
20
10
0
20
4100-S
4100S-205
4100S-210
4100S-224
4100S-248
pure Mg
4125HA-225
3801S-205
3810S-205
30
4
0
0
40 0
0
5
Group B
35
2
10
as-cast
3805-H
3810-H
4100-S
70
12
80
Group A
ev
14
30
4100-S20
4100S-205
4100S-210
4100S-224
4100S-248
pure Mg
40
60
80
100
40
60
80
100
40
60
80
100
Group B
25
20
15
10
5
0
0
0
10
20
30
4100-S
pure Mg
4
0
0
5
40
4100-S20
pure Mg
20
35
4
30
25
20
15
10
5
0
0
0
10
20
30
40
50
immersion time, h
(a) 48 h immersion
immersion time, h
(b) 96 h immersion
Fig. 6. Hydrogen evolution for the various microstructures during immersion in 1 N NaCl for the stated period.
dure has removed negligible Mg metal and (iii) that there was
negligible weight change of the encapsulating epoxy resin due to
exposure to the 1 N NaCl solution or to the acid cleaning solution.
3.9. Macroscopic corrosion morphology
The corrosion of AZ91 initiated as localized corrosion at some
sites on the surface and subsequently expanded over surface. The
advance of the corrosion over the surface was different for different
conditions. At the end of the 48 or 96 h immersion time, the active
corrosion area was covered by a thick layer of corrosion products
and was different for the various conditions as presented by the
macro-photographs (27 mm 18 mm) in Figs. 9 and 10. In most
cases, the area corroding after 96 h immersion was larger than
after 48 h immersion.
In marked contrast to the local corrosion of AZ91, the corrosion
for pure Mg immersed in 1 N NaCl was uniform corrosion; there
48 h immersion
HA3805
6
5
HA4105
4
HA4110 HA4125
SA248
as-cast
SS
2
SA210
SA224
4125HA225
SA205
3801S205
3810S205
pure Mg
0
1
20
4HA3810
5
10
11
13 14 15
9612h immersion
15
HA3805
SS
10
SA248
as-cast
SA224
5
SA205
SA210
pure Mg
0
1
Fig. 7. Weight loss data for the various microstructures during immersion in 1 N
NaCl for the stated period.
48 h
96 h
Y=1.085X
20
15
10
0
0
10
20
30
1947
4. Discussion
1948
Fig. 9. Macro-appearance (27 mm 18 mm) of the corrosion morphology after 48 h immersion for different microstructures.
much faster than that on the surface of the a-phase and thus the bphase is a more effective cathode [14]. A competition between micro-galvanic corrosion and the corrosion barrier effect can explain
the corrosion [14]. If the b-phase is present as a small fraction,
the b-phase serves mainly as a galvanic cathode and accelerates the
overall corrosion of the a matrix. If b-phase fraction is high, the bphase may act mainly as a barrier against the corrosion of the a matrix. In the as-cast condition, Fig. 11 shows that the
a-Mg matrix adjacent to coarse b particles with lack of the surrounding lamellae (a + b) eutectic has undergone the majority of
the corrosion, with there being less corrosion of the b particles
and the ne lamellar a + b micro-constituent. The corrosion is initiated and gradually advanced by the dissolution of the a-Mg matrix
adjacent to the region of the continuous lamellar micro-constituent
plus coarse b particles. When the propagation of the corrosion attack reaches the region of the continuous (a + b) micro-constituent
plus coarse b particles, the corrosion is retarded to a certain extent
as shown in Fig. 11. In this case, even though the a-Mg matrix surrounding the (a + b) plus coarse b particles is corroded, some should
be under the continuous lamellae (a + b) plus coarse b particles as
the a-Mg matrix in the top layer has corroded. In fact, the corrosion
damage as above-mentioned is quite common for AZ91D in a corrosive environment. There is evidence for some b particles being
undermined from corroding areas of AZ91D under an atmospheric
corrosion [28].
Section 3.1 evaluated the formation of the ne lamellar (a + b)
micro-constituent. This evaluation led to the realisation that a
1949
Fig. 9 (continued)
1950
Fig. 10. Macro-appearance (27 mm 18 mm) of the corrosion morphology after 96 h immersion for different microstructures.
1951
Fig. 12. Typical corrosion morphology for HA3805 and HA4110 conditions for metallographic polished specimens; arrows indicate isolated ne b particles.
1952
5. Conclusions
1. The ne lamellar (a + b) micro-constituent, in as-cast AZ91,
may be nucleated by a b-phase plate. This b-phase plate may
be effective as a corrosion barrier to subsequent corrosion.
2. Most AZ91 specimens exhibited an increase in corrosion rate
with increasing immersion time for immersion times of up to
96 h in 1 N NaCl. Part of the reason for the increasing corrosion
rate is the increase in area corroded with increasing immersion
time. This means that long term immersion tests lasting two
weeks to a month may be needed to measure steady state corrosion rates.
3. Relatively short immersion tests like 48 h are valuable as they
reveal the same trends as longer immersion tests 96 h, and
most probably also correlate with steady state corrosion
conditions.
4. The weight loss rate is directly related to the hydrogen evolution
rate by the relationship: weight loss rate [mg/cm2/d] = 1.085
(Hydrogen evolution rate [ml/cm2/d]), as expected from the
overall magnesium corrosion reaction that one molecule of
hydrogen is evolved for each atom of corroded magnesium.
5. There was considerable difference in corrosion rates and areas
corroded for the various microstructures.
6. AZ91SS (i.e. AZ91 subjected to a solid solution heat treatment of
100 h at 410 C and water quenched to have a microstructure
largely single a-phase) had a corrosion rate higher than that
of pure Mg despite the fact that the corrosion covered part of
the surface for AZ91SS whereas corrosion was uniform for pure
Mg and covered the whole surface of the pure Mg. Thus the
higher corrosion rate for AZ91SS is not an effect of surface area
corroding. An impurity explanation is ruled out by the fact that
both AZ91 and pure Mg were high purity.
Acknowledgements
This work was supported by the ARC Center of Excellence, Design of Light Alloys. CAST CRC was established under, and is supported in part by, the Australian Governments Cooperative
Research Centres scheme. DH StJohn is thanked for valuable discussion on the formation of the ne lamellar (a + b) microconstituent.
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