J. Cent. South Univ.

(2018) 25: 961−975

DOI: https://doi.org/10.1007/s11771-018-3797-5

Effect of annealing treatment on microstructure and

fatigue crack growth behavior of Al–Zn–Mg–Sc–Zr alloy

CHEN Jing(陈婧)1, PAN Qing-lin(潘清林)1, YU Xue-hong(虞学红)1, LI Meng-jia(李梦佳)1,

ZOU Hao(邹浩)1, XIANG Hao(向浩)1, HUANG Zhi-qi(黄志其)2, HU Quan(胡权)2

1. School of Materials Science and Engineering, Central South University, Changsha 410083, China;
2. Guangdong Fenglu Aluminum Co., Ltd, Foshan 528000, China
© Central South University Press and Springer-Verlag GmbH Germany, part of Springer Nature 2018

Abstract: Al–Zn–Mg–Sc–Zr alloy samples were annealed to four different states (under-aging, peak-aging, over-aging
and double-aging) and then thoroughly investigated by means of electron backscatter diffraction (EBSD), transmission
electron microscopy (TEM), scanning electron microscopy (SEM), tensile and fatigue crack growth rate tests to explore
the influence of annealing treatment on microstructure and fatigue crack growth behavior. The results indicate that
Al3(Sc,Zr) particles can effectively refine grains and enhance tensile properties and fatigue properties. After annealing
treatment, the under-aged sample and double-aged sample obtained average grain sizes of 4.9473 and 4.1257 μm, and
the maximum value of yield/tensile strength (561 MPa/581 MPa) was obtained in peak-aged state. In the Paris region,
fatigue crack growth rate, crack deflection and bifurcation, crack blunting and inter/trans-granular propagation were
discussed based on data fitting and Laird model and Griffith theory. And the results show that the under-aged sample
possesses the best resistance to fatigue crack propagation and the most tortuous and bifurcated crack path. For all
samples, the fatigue crack growth rate in the rupture region was inversely proportional to yield strength.

Key words: Al–Zn–Mg–Sc–Zr alloy; annealing treatment; microstructures; fatigue crack growth rate; fatigue crack
path

Cite this article as: CHEN Jing, PAN Qing-lin, YU Xue-hong, LI Meng-jia, ZOU Hao, XIANG Hao, HUANG Zhi-qi,
HU Quan. Effect of annealing treatment on the microstructure and fatigue crack growth behavior of Al–Zn–Mg–Sc–Zr
alloy [J]. Journal of Central South University, 2018, 25(5): 961–975. DOI: https://doi.org/10.1007/s11771-018-3797-5.

formation of unstable microstructures [4, 5].

1 Introduction Artificial aging has been traditionally applied to
enhance the strength of Al–Zn–Mg alloys on
The age hardenable Al–Zn–Mg alloys, account of fine and uniformly distributed
benefiting from their high strength/weight ratio and precipitates MgZn2 in the matrix [6–8]. However,
stiffness, have been widely used in aerospace higher strength obtained by heat treatment is gained
manufacturing and other transportation applications at the price of lower toughness [9]. Inverse
[1–3]. As we all know, the common methods of correlations between strength and ductility, strength
strengthening aluminum alloys are strain hardening and fracture toughness are repeatedly found.
and heat strengthening. However, strain hardening As the aerospace technology develops at an
also leads to poor ductility and may cause the incredible speed, aluminum alloys with higher
Foundation item: Project(2012CB691503) supported by the National Key Basic Research and Development Program of China;
Project(2016B090931001) supported by Science and Technology Program of Guangdong Province, China
Received date: 2016−11−11; Accepted date: 2017−02−22
Corresponding author: PAN Qing-lin, PhD, Professor; Tel: +86–731–88830933; E-mail: qinglinpan_CSU2016@163.com
962
strength and toughness are in badly need. A number
of researches about micro-alloying have been
conducted to further enhance the mechanical
performance of Al–Zn–Mg alloys. Among dozens
of micro-alloying elements, the combination of Sc
and Zr is considered to be one of the most effective
elements due to the fact that the coherent Al3(Sc,Zr)
precipitates can effectively inhibit grain growth and
prevent the motion of dislocations [10, 11]. It has
been reported that Sc and Zr can also interact with
aluminum separately to form Al3Sc and Al3Zr
precipitations, but the Al3Zr precipitation always
exhibits disordered distribution for the segregation
of Zr during solidification, while the Al3Sc phase
can disperse uniformly for its higher solubility
[12–15]. PEREZ et al [11] and ROBSON et al [15]
confirmed that the disordered distribution of Al3Zr
precipitates can be remedied by the faster
nucleating Al3Sc precipitates by forming a finer and
dispersive Al3(Sc,Zr) phase. RIDDLE et al [16]
found that alloys containing both Sc and Zr show
even better recrystallization resistance than either
addition of Sc or Zr. Moreover, Sc is more costly
than Zr, which restricts the commercial application
of Al–Sc alloys. Consequently, the combination of
Sc and Zr is applied in this work. Numerous
researches have concentrated on the precipitation
behavior of Al3(Sc,Zr) particles and their grain
refining effect. The effect of varied amount of Sc
addition on microstructure and mechanical
properties of Al–Zn–Mg–Zr alloy has been studied
in our previous work [17]. The result showed that
the optimal amount of Sc is 0.25% (wt%), which
can obtain the finest grain size. ZHAO et al [18]
also indicated that the addition of Sc contributes
considerably in enhancing tensile strength and
ductility, as Sc can influence the morphology of the
primary α-Al in the slurry.
The fatigue failure is known to be one of the
main destruction causing air crashes [19–21].
Unfortunately, the fatigue resistance of aluminum
alloys is usually poor. Therefore, the study on
fatigue properties of aluminum alloys is necessary.
As a result, fatigue crack growth behavior and
fatigue life prediction became quite heated in recent
years. Fatigue crack growth rate, the most
commonly used indicator to characterize the fatigue
properties of alloys, can be described by the
da/dN–ΔK curve which can be divided into three
regions and the Paris law has been widely accepted
J. Cent. South Univ. (2018) 25: 961–975
to describe the relation of fatigue crack growth rate
da/dN and applied stress intensity factor range ΔK
in the second region [22]. Many models have been
proposed to illustrate the process in the Paris region
such as the slip band extrusion intrusion model,
dislocation blocking model and crack tip blunting
and resharping model. However, none of them can
explain the fatigue behavior of precipitation
hardened aluminum alloys. It is generally agreed
that heat treatment has significant influence on the
fatigue properties as different microstructures can
lead to different crack propagation behaviors [23].
Various heat treatments have been extensively
studied to explore the effect of heat treatment on
fatigue behavior [19, 24–27]. As early as the 1930 s,
OROWAN [19] reported that metastable
precipitates in peak-aged aluminum alloys will turn
to over-aging state even at room temperature during
cyclic deformation, resulting in a degradation of
mechanical performance. Recently, in HAN’s
reports [25] and HUTCHINSON’s [24], profuse
dynamic precipitations of aluminum alloys were
observed during the process of cyclic deformation
at room temperature. The volume fraction of GP
zone increased in the under-aged states, and it was
found that under-aged aluminum alloys exhibited
longer fatigue life compared with the peak-aged
ones. WANG et al [26] revealed that retrogression
and reaging treated Al–Zn–Mg–Cu alloy, benefiting
from its precipitates in the matrix and the narrower
PFZs, demonstrated better fatigue property than
T7451.
However, previously reported studies mainly
focused on the fatigue performance of Al–Zn–Mg–
Sc–Zr alloys under different heat treatments. The
present work performs a detailed analysis on crack
propagation process from microscopic view. And
the effect of different annealing treatments on the
microstructure and fatigue crack growth behavior of
studied alloy is also thoroughly investigated. These
results may offer useful information for optimizing
the heat treatment system for industrial applications,
and will be necessary for establishing a crack
propagation mechanism for Al–Zn–Mg–Sc–Zr
alloys.
2 Experimental procedures
2.1 Material
Base metal used in the experiment was
J. Cent. South Univ. (2018) 25: 961–975
Al–Zn–Mg–Sc–Zr alloy, which was cast via
metallurgy with pure Al, Zn, Mg metals and Al–Cu,
Al–Mn, Al–Sc, Al–Zr master alloys into 260 mm×
150 mm×30 mm ingots. Table 1 shows its chemical
composition. The specimens were taken from the
middle of the ingot and homogenized at 470 °C for
24 h. Then a hot rolling process was applied to
5.7 mm (77% rolling reduction) at 470 °C, which
was followed by intermediate annealing at 420 °C
for 1 h. Subsequently, the hot-rolled sheets were
cold-rolled to a thickness of 2.0 mm (65%
reduction). The cold-rolled sheets were subjected to
solid solution treatment at 470 °C for 1 h, followed
by water quenching, and then the specimens were
aged at 120 °C for 4 h (under-aged sample,
designated as UA), 24 h (peak-aged sample,
designated as PA), 48 h (over-aged sample,
designated as OA), and 120 °C for 6 h then 140 °C
for 20 h (double-aging, designated as DA),
respectively.
Table 1 Chemical composition of Al–Zn–Mg–Sc–Zr
alloy (mass fraction, %)
Zn Mg Cu Mn Sc Zr Al
5.40 2.00 0.35 0.30 0.25 0.10 Bal.
2.2 Tensile and fatigue crack growth rate tests
The tensile tests were conducted on MTS-858
tester. Specimens were taken from the plates in the
longitudinal transverse direction according to
ASTM E647 standard. For each sample, three
tensile specimens were tested and the average value
of the results was adopted to evaluate the strength
and ductility of the sample.
Fatigue crack growth tests were carried out on
a MTS-810 test machine using middle-tension (MT)
specimens according to ASTM E647 standard.
Figure 1 shows the major dimensions of the sample
Figure 1 Geometry of MT specimen (dimensions in mm)
963
used in the tests. All the tests were conducted in air
at room temperature, with a stress ratio (Pmin=
1.4 kN, Pmax=14 kN, R=Pmin/Pmax) of 0.1 and a
sinusoidal loading which was applied at a frequency
of 10 Hz. The length of fatigue crack was measured
by an optical microscope (±1 μm) attached on the
fatigue machine. The following equation was used
to determine the stress intensity factor ΔK:
P π π
K  sec (1)
B 2w 2
where P is the load (in MPa); B and w are the
thickness (in mm) and the width of the sample,
respectively; α=2ɑ/w, and ɑ is the half-crack length
(in mm).
2.3 Microstructural analysis
To characterize the microstructure of samples
detailedly, the transmission electron microscopy
(TEM) was utilized. The tested thin foils were
prepared by twin-jet electro-polishing at 20 V in a
solution consisting of 30% nitric acid and 70%
methanol (vol.%) at –25 °C and observed on a
TECNAI G2 F20 electron microscope, with an
acceleration voltage of 200 kV.
The fatigue fracture surfaces and crack
propagation paths were analyzed on FEI QUANTA-
200 and Helios scanning electron microscopy
(SEM).
To explore the crystallographic relationships
between fatigue crack path and the subgrain
morphology and orientation, electron backscattered
diffraction (EBSD) methods was implemented with
an accelerating voltage of 20 kV.
3 Results and discussion
3.1 Microstructure characterization
As shown in Figure 2, orientation distribution
964
of the grains with the crack were measured by
EBSD analysis accessory. Different orientations of
the grains are marked by different colors and the
EBSD inverse pole-figure (IPF) map superposed
with the grain boundary (GB) component of the
crack reveals the grain structure. The high angle
boundary (>15°) and low angle boundary
(2°<θ<15°) are delineated by lines in different
colors. The misorientation angle distribution and
grain size statistics are shown in Figure 3.
According to the results, the average misorientation
angles of the UA sample and DA sample are
27.709° and 27.336°, and the average grain sizes
are 4.9473 μm and 4.1257 μm, respectively. WANG
et al [26] and WEI et al [28] studied the mechanical
properties and fatigue fracture behavior of
Al–5.67Zn–1.92Mg–1.89Cu alloy with different
heat treatments, and its composition is close to that
of the alloy used in this work except the present
alloy containing a small amount of Sc and Zr. The
average grain size of Al–5.67Zn–1.92Mg–1.89Cu
alloy after aging treatment was about 50 μm, nearly
13 times ours, which proves that the addition of Sc
resulted in a good recrystallization resistance.
There is no significant change of structural and
grain size between samples under different
Figure 2 EBSD observations of fatigue crack behavior in Paris region: (a) UA sample; (b) DA sample
J. Cent. South Univ. (2018) 25: 961–975
annealing treatments in EBSD analysis (Figure 2).
Therefore, the TEM observation was applied to
further explore the detail microstructure inside
grains. It is widely accepted that the precipitation
sequence of Al–Zn–Mg–Cu series aluminum alloys
is showed as followings: supersaturated solid
solution (α)→GP zone→metastable η′→
equilibrium η (MgZn2) [7, 29]. GP zone is atom
clustering zone which is coherent with α(Al) matrix.
The η′ phase is a metastable hexagonal phase and is
semi-coherent with α (Al) matrix. The η phase is an
equilibrium phase and is non-coherent with α (Al)
matrix. And Al3(Sc,Zr) precipitate, the most
important type of precipitates in this work, is
coherent with α(Al) matrix [30–32]. These
Al3(Sc,Zr) precipitates, dispersing in the grains and
at the grain boundaries, can pin dislocations and
grain boundaries, resulting in better resistance of
mechanical properties[29].
Figure 4 shows the TEM images of the
samples with different annealing treatments. For the
UA sample (Figures 4(a) and (b)), no obvious
precipitates can be found in the grains, and the
grain boundaries were continuous. The inset image
in Figure 4(b) is the SAED pattern of the UA
sample obtained by projecting along the [011] Al
J. Cent. South Univ. (2018) 25: 961–975
Figure 3 Misorientation angle distribution and grain size statistics: (a, b) UA sample; (c, d) DA sample
orientation. The diffraction spots from α(Al) matrix
have been indexed, and those spots marked by the
white arrows are derived from Al3(Sc, Zr) particles
with a Ll2 cubic crystal structure. For the PA sample,
a large quantity of precipitates distribute
homogenously in the grains, and the precipitates in
grain boundaries are more apparent and coarser as
shown in Figures 4(c) and (d). The precipitation
free zone (PFZ) can also be observed, and its small
width indicates that it was just formed during this
process. As the sample was aged to OA and DA
states (Figures 4(e) and (f)), the precipitates in the
grain grew lager and the η precipitates coarsened
and became completely discontinuous along the
grain boundaries. Meanwhile, the precipitation free
zone (PFZ) broadened. Compared with DA sample,
the precipitates inside the grains of OA sample are
more unevenly dispersed and the precipitates in
grain boundaries are more discontinuous and
coarser. Petal-shaped Al3(Sc,Zr) precipitates can be
observed in all samples (Figure 4). Around the
particles, a large number of dislocations and
dislocation tangles were observed, which proves
that Al3(Sc,Zr) precipitates can pin the dislocation.
965
In order to investigate the evolution of these
particles during annealing treatment, two TEM
images were selected randomly to calculate the
average size of Al3(Sc,Zr) particles for each sample.
Results show that the average equivalent diameters
of Al3(Sc,Zr) particles are 29.1 nm for UA sample,
28.9 nm for PA sample, 29.3 nm for OA sample,
and 29.4 nm for DA sample.
In conclusion, with the degree of aging
treatment increasing, the precipitates in the grains
became more apparent, which illustrates that GP
zones gradually transferred into uniformly
dispersed η′ phases and the η′ phase transferred into
coarser η phase. The grain boundary also became
more and more discontinuous and the PFZ
broadened. Meanwhile, the nucleation and growth
of GP zones and η′ phase became much more
apparent. The size of Al3(Sc,Zr) particles generally
remains unchanged with an averaged diameter of
about 29 nm.
3.2 Mechanical properties
Table 2 shows the tensile properties of the
studied samples. It can be clearly observed that the
966 J. Cent. South Univ. (2018) 25: 961–975

Figure 4 TEM micrographs of Al–Zn–Mg–Sc alloy with different annealing treatments: (a,b) UA sample (the inset is
the SAED pattern); (c, d) PA sample; (e, f) OA sample; (g, h) DA sample
J. Cent. South Univ. (2018) 25: 961–975 967

Table 2 Tensile properties of Al–Zn–Mg–Sc–Zr alloys

Tensile Yield
Elongation,
Specimen strength, strength,
A/%
Rm/MPa Rp/MPa
Annealed at 120 °C for
548 524 12.2
4 h (UA)
Annealed at 120 °C for
581 561 11.1
24 h (PA)
Annealed at 120 °C for
577 549 10.9
48 h (OA)
Annealed at 120 °C for
6 h and at 140 °C for 548 527 12.3
20 h (DA)

tensile strength increases first and then decrease

slightly with the degree of aging treatment
increasing. And the ultimate tensile strength of
581 MPa and yield strength of 561 MPa are
obtained for the PA sample. The tensile properties
of UA sample are close to those of DA sample, and
both of them are lower than samples in PA and OA
states.
Compared with the properties of peak-aged
Al–Zn–Mg–Cu in Ref. [26], the tensile strength and
yield strength of peak-aged Al–Zn–Mg–Sc–Zr in
this work are 21 MPa and 56 MPa higher,
respectively. This improved performance can be
attributed to the countless uniformly dispersed fine
Al3(Sc,Zr) precipitates in the grains, which can be
clearly observed in Figure 4. These Al3(Sc,Zr)
precipitates were not only uniformly dispersed but
also coherent with the Al matrix, which enabled
them to contribute to stabilizing the fine grained
microstructure and strengthen the alloys by pinning
the grain boundary and hindering the dislocation
motion [33].
The fatigue crack growth rates da/dN vs
applied stress intensity factor ranges ΔK of samples
with different annealing treatments are compared.
In the double logarithmic plot of da/dN against ΔK
is shown in Figure 5, in which the da/dN–ΔK curve
can be divided into three regions, the threshold
region, the Paris region and the rupture region.
As Figure 5(a) shows, the UA sample
possesses a wider range of ΔK than the PA state.
And when ΔK<30 MPa·m1/2, the UA sample
exhibits a higher resistance to fatigue crack
propagation as compared with the PA sample. But
when ΔK>30 MPa·m1/2, the fatigue crack grew more
quickly in the UA sample than in the PA sample.
Figure 5(b) illustrates that the curves of OA and DA
samples are almost identical in the first two regions.
Figure 5 Double logarithmic plots of da/dN against ΔK:
(a) UA sample and PA sample; (b) PA sample and DA
sample
The fatigue crack propagation resistance of DA
sample is slightly higher than that of OA sample.
However, when ΔK>27 MPa·m1/2, the curve of DA
sample shows a typical curving shape and its crack
expanding speed increases more quickly. And the
curve of DA sample exhibits a wider range of ΔK
than the OA one.
To quantify fatigue properties of four samples
and analyze them more accurately, data fitting of
the Paris region is necessary. The Paris region is the
linear region in the double logarithmic plot of
da/dN against ΔK, which can be described by the
following equation:
da
 C (K ) m (2)
dN
where m is the Paris exponent and C is the Paris
constant. The values of these two constants (C and
m) can be obtained by data fitting for the Paris
region of the plot. The fitted lines are displayed in
Figure 6, and the calculated values along with the
corresponding fracture cycle numbers are listed in
Table 3. According to the results, the DA sample
has smaller C and m than the OA sample, which
indicates that the DA sample possesses better
968 J. Cent. South Univ. (2018) 25: 961–975

Figure 6 Logarithm of fatigue crack growth rate as a function of logarithm stress intensity factor range: (a) UA sample;
(b) PA sample; (c) OA sample; (d) DA sample

Table 3 Fitting results and total cycle numbers of sample are wider than those of samples in UA and
samples OA states, which is in good agreement with the
Sample C m Cycle number result of range of samples’ ΔK (Figure 5).
UA 3.1445×10 –5
0.9649 81487 Obviously, the fatigue crack path of the UA sample
–5 is the most tortuous while the PA one is the
PA 6.1210×10 0.88668 65066
–5
straightest. The OM image in Figure 7(c) shows the
OA 7.5502×10 0.79109 72238
–5
crack tip of UA sample at ΔK=22.157 MPa·m1/2,
DA 5.9895×10 0.7647 75189
which evidences significant crack deflection and
branching.
resistance to fatigue fracture. Although the value of To explore the crystallographic relationships
m of UA sample is slightly larger than that of PA between fatigue crack path and the grain
sample, the value of C of PA sample is as twice as morphology and orientation, EBSD observations
the UA sample’s. Hence, it can be concluded that (Figure 2) were applied on UA sample and DA
the UA sample has the best resistance to fatigue sample to investigate the differences of their fatigue
fracture and the PA sample is the poorest. The propagation in Paris region. Second cracks can be
analysis of fitting result is in good agreement with clearly observed in both samples. As is well known,
the da/dN–ΔK curves and the total cycles. crack propagations can be classified into
inter-granular mode and trans-granular mode, and
3.3 Fatigue crack path the crack tends to deflect when entering into a new
The digital images of fracture surfaces and grain. However, the crack path deflected even
side views are shown in Figure 7 and the fatigue within the grain in the present results. By analyzing
crack growth area is marked by red lines. The the EBSD result of the UA sample, it can be
fatigue crack growth area of PA sample and DA concluded that both the lead crack and the second
J. Cent. South Univ. (2018) 25: 961–975 969

Figure 7 Photos of fracture surfaces (a) and side view of crack paths (b) and OM image crack path of UA sample (c)
970
crack present a trans-granular propagation mode.
For the DA sample, the crack still mainly presents a
trans-granular extension, but inter-granular cracks
can also be observed both in the master crack and
second cracks (marked by black ellipses), which
differs from the UA sample.
In order to investigate the interaction of fatigue
crack with particles, SEM and EDS techniques are
employed in the analysis of UA sample. As shown
in Figure 8(a), the fatigue crack cut the impurity
particles and advanced into the alloy matrix, which
can be proved by the small fragments left in the
crack. However, branching crack observed in
Figure 8(b) can be attributed to the deflecting and
retarding effect by Al3(Sc,Zr) particles.
The impediment caused by particles is an
important factor in fatigue crack growth behavior.
The Griffith theory holds that a flaw will propagate
in a stressed material only when it brings about a
reduction in elastic stored energy more than
sufficient to meet the free energy requirements of
the newly formed fracture surfaces [21]. The critical
stress required to propagate the crack is given by
Figure 8 Interaction of fatigue crack with particles of alloy and corresponding EDS patterns: (a) Crack cutting by Fe
particle; (b) Crack deflections caused by Al3(Sc,Zr) particle
J. Cent. South Univ. (2018) 25: 961–975
the Griffith equation:
1
 2 E  2
c    (3)
 πa 
where E is elastic modulus; γ is the surface energy
(per unit area) and a is the half-crack length.
According to the Griffith theory, the extension
stress at the crack tip would be increased when the
fatigue crack tip encounters particles that can be
broken easily. Once these particles are broken, the
crack will propagate a longer distance than that in a
region without stress concentration (Figure 8(a)). In
other words, the easily broken particles reduced the
critical stress, which results in a sensitive resistance
to fatigue crack propagation.
Oppositely, when the crack tip encountered
particles that only can be bypassed, like the η phase
and Al3(Sc,Zr) particle, it stagnated momentary and
then bypasses these particles because the stress is
insufficient to break the particles and propagate on
(Figure 8(b)). Therefore, the crack propagation was
hindered by such particles.
J. Cent. South Univ. (2018) 25: 961–975
3.4 Fatigue fractographic analysis and
mechanism analysis
To validate the fatigue properties of the
samples further and explore their mechanism at the
micro level, fractographs of the Paris region and the
rupture region were investigated. Figure 9 displays
the fractographs of samples in Paris region
(ΔK=22.157 MPa·m1/2), and all of the fractures
show the typical characteristics of striations. The
average striation distance and the corresponding
fatigue crack growth rate of each sample are shown
in Table 4. As is well known, every fatigue cycle
produces a fatigue striation in Paris region [34].
That is to say, the narrower the fatigue striation
distance is, the slower the fatigue crack grows,
which indicates a better resistance to fatigue
propagation. Besides, second cracks inside the grain
can be clearly observed in the UA sample (Figure
9(a)), which grew perpendicular to the direction of
the lead cracks. Second cracks can also be found in
DA sample (marked by arrows in Figure 9(d))
although it is along the grain boundary and slighter.
In general, the distance of striation is strictly
proportional to the crack propagation rate, but in
this work this strictly proportional relationship is
broken due to the presence of second cracks, which
can increase the total crack path. Thus, the slight
Figure 9 SEM images of samples in Paris region at condition of ΔK=22.157 MPa·m1/2: (a) UA sample; (b) PA sample;
(c) OA sample; (d) DA sample
971
fluctuation of the ratios between striation width and
crack propagation rate is reasonable, and the results
are in good agreement with the measured crack
propagation rates (Figure 5) and the fitting results
(Table 3).
Generally speaking, the fracture of metals is
governed by localized deformation that leads to a
very poor macroscopic ductility and dimpled
fracture surfaces [35]. Figure 10 shows the
fractographs in rupture region of these four samples.
The presence of countless dimples indicates that all
samples had showed a good quality of ductility and
their main failure mode was ductile trans-granular
mode. Compared with UA sample, PA and OA
samples (Figures 10(b) and (c)) have much smaller
and more intensive dimples due to prolonged
annealing treatments, which is the evidence of
higher strength. Additionally, their tear ridges are
more obvious. Notably, inter-granular failure along
grain boundaries can be observed in OA sample
occasionally (pointed out by red arrows), which
may explain its higher fatigue crack propagation
rate in rupture region. And finally, for the DA
sample, its fracture surface possesses the largest
dimples, which explains its better elongation. And
tear ridges on its fracture surface are even more
obvious compared with those of the others. For all
972 J. Cent. South Univ. (2018) 25: 961–975

Table 4 Fatigue crack growth data and close when unloaded, resulting in the formation
Sample at Striation (da/dN)/ of a fatigue strip with each tensile loading.
ΔK=22.157 MPa·m1/2 width/nm (mm·cycle–1) According to the Laird model, it can be deduced
UA 313.1 6.13×10–4
that the fatigue crack propagation rate is inversely
PA 750.6 1.10×10–3 proportional to the yield strength. However, just
OA 468.1 9.05×10–4 like numerous researches reported, the present
DA 357.5 8.03×10–3 results do not totally follow this rule.
Actually, since aluminum alloy is a ductile
samples, many aggregates of second phase particles material, its elasticity will lead to the closure of
can be observed at the bottom of dimples, which crack tip when the high stress loading suddenly
indicates that coarse particles may facilitate the drops to a low stress, which explains the formation
formation of dimples. Overall, it can be concluded of strips during cyclic loading of tensile stress.
that the result of fractographs analysis in rupture Moreover, as the crack propagation goes, the crack
region is in good agreement with the tensile tip grows faster due to increasing stress intensity
properties. (ΔK). When the maximum stress exceeds the yield
To explain the fatigue crack behavior, many strength, the crack tip opens quickly and grows
models have been built based on crystal plasticity. larger, then the effect of crack tip closure becomes
However, the processes and mechanisms involved invalid, resulting in the unstable propagation
in fatigue fracture are too complicated that no process. During this process, the crack propagation
model can explain all the fatigue behaviors in rate increases quickly and ends up with fracture
different conditions until now. It is now accepted when the stress reaches the tensile strength. Simply
that different microstructures can lead to different stated, based on the above discussion, the inversely
crack propagation behavior. In general, the fatigue proportional relationship between yield strength and
crack propagation rate is intimately bonded to yield fatigue crack growth rate only stands in the rupture
strength of materials. The crack tip plastic blunting region. Moreover, with a higher yield strength, the
model put forward by LAIRD et al [36] supports ΔK needed for arousing the rupture region will be
the idea that the crack tip will open under loading higher, and the fatigue crack will grow slower. And

Figure 10 SEM fractographs of samples in rupture region: (a) UA sample; (b) PA sample; (c) OA sample; (d) DA
sample
J. Cent. South Univ. (2018) 25: 961–975
in this study, results of fatigue crack growth rate in
rupture region conformed this point. The PA sample
possesses a higher yield strength, which is
responsible for the wider Paris region and lower
fatigue crack growth rate when ΔK>30 MPa·m1/2.
Similarly, compared with DA sample, the fatigue
crack growth rate of OA sample in rupture region is
lower owing to its higher yield strength.
The results of crack path in EBSD analysis
(Figure 2) demonstrate that the trans-granular mode
is the main way of the crack propagation in Paris
region, so optimizing the microstructure inside the
grains is an important method to improve the
fatigue properties of alloys. Numerous studies have
showed that precipitation hardened aluminum
alloys would experience profuse dynamic
precipitations inside the grains when they were
subjected to cyclic deformation due to the
instability of the precipitates’ microstructure [19, 24,
25]. Similarly, in this work, as the cyclic
deformation goes, the metastable η′ phase formed in
PA sample will gradually turn to over-aging state η
phase, whose strengthening effect is weaker than
the former one. While in the UA sample, the GP
zone formation is accelerated during the cyclic
deformation. Thus, the cyclic deformation will
result in a degradation in the mechanical
performance for the PA sample and a promotion for
the UA sample. Moreover, crack branching and
deflection are also unneglectable factors. The
fractographs of crack paths and side views
(Figure 7) illustrate that fatigue crack path in UA
sample is more tortuous and bifurcated, which can
greatly reduce the fatigue crack growth rate. Based
on the above points of view, the superiority of
fatigue properties of UA sample can be explained.
As shown in Figure 2(b), the wide PFZ
adjacent to the grain boundary in the DA sample
leads to its inter-granular crack propagation to some
degree. There are two opposite theories about the
effect of PFZ on mechanical properties. One theory
believes that the PFZ is mechanically weaker than
the matrix due to its depletion of solute. The other
one holds that PFZ is so soft that it enhances the
toughness. The results of the present work support
that the second one is more suitable for the current
fatigue behavior considering the crack blunting.
Since the PFZ is almost equivalent to the pure
matrix, it is soft enough to relax the stress when the
crack tip enters, and it is also beneficial to crack
973
blunting as it can retard the propagation. Therefore,
the DA sample possesses a wider Paris region
despite of its lower yield strength.
However, compared with the DA sample, the
OA sample with the same wide PFZ exhibits a
narrower Paris region. This can be explained by
their microstructure differences as follows. For the
DA sample, it was reported before that the large
size and stable GP zone will be formed after
pre-aging treated at 120 °C [7]. Then, the η′ phase
nucleates and grows at effective GP zone formed
before during the final aging at 140 °C. Hence,
compared with those of the OA sample, the
precipitates inside the grains of DA sample are
more uniformly dispersed, which is the reason of its
better fatigue properties. Moreover, the precipitates
at the grain boundary of OA sample are more
disordered and coarser than those of DA sample
(Figure 4), resulting in higher fatigue crack growth.
And this negative effect depleted the benefit
brought by the PFZ.
4 Conclusions
The effect of annealing treatment on the
microstructure and fatigue crack growth behavior of
Al–Zn–Mg–Sc–Zr alloy has been investigated. The
following results can be concluded:
1) During the aging treatments, the size of
Al3(Sc,Zr) particles keeps unchanged, maintaining
an average diameter of about 29 nm. And these
Al3(Sc,Zr) particles bring about a remarkable grain
refining effect that for UA sample and DA sample
average grain sizes of 4.9 and 4.1 μm are obtained,
respectively. Besides, they also impede and deflect
the fatigue crack propagation by pinning up the
dislocations, greatly improving the tensile
properties and fatigue properties.
2) Among these four samples, the UA sample
exhibits the best fatigue properties, whose crack is
most bifurcated and deflects and propagates
trans-granularly through the grains.
3) Compared with the OA sample, DA sample
shows better fatigue properties, which can be
attributed to its more uniformly dispersed
precipitates in the grains and more continuously
distributed finer precipitates at the grain boundaries.
This work also confirms that the wide PFZs in both
DA and OA samples are soft enough to release the
stress and arise crack blunting, resulting in
974
improved fatigue properties.
4) This work proves that the inversely
proportional relationship between yield strength and
fatigue crack growth rate is only tenable in the
rupture region.
References
[1] ZHANG Li-hua, YU Jun, ZHANG Xiao-ming. Effect of
ultrasonic power and casting speed on solidification structure
of 7050 aluminum alloy ingot in ultrasonic field [J]. Journal
of Central South University of Technology, 2010, 17:
431–436.
[2] WILLIAMS J C, STARKE E A. Progress in structural
materials for aerospace systems [J]. Acta Materialia, 2003,
51(19): 5775–5799.
[3] DURSUN T, SOUTIS C. Recent developments in advanced
aircraft aluminium alloys [J]. Materials & Design, 2014, 56:
862–871.
[4] YAN Liang, DU Feng-shan, DAI Sheng-long, YANG
Shou-jie. Effect of age condition on fatigue properties of
2E12 aluminum alloy [J]. Journal of Central South
University of Technology, 2010, 17: 697–702.
[5] MORRIS D G, MUNOZ-MORRIS M A. Microstructure of
severely deformed Al-3Mg and its evolution during
annealing [J]. Acta Materialia, 2002, 50(16): 4047–4060.
[6] SMOLA B, STULÍKOVÁI I, OČENÁŠEK V, PELCOVÁ J,
NEUBERT V. Annealing effects in Al–Sc alloys [J].
Materials Science and Engineering A, 2007, 462(1, 2):
370–374.
[7] SHI Yun-jia, PAN Qing-lin, LI Meng-jia, HUANG Xing, LI
Bo. Influence of alloyed Sc and Zr, and heat treatment on
microstructures and stress corrosion cracking of
Al–Zn–Mg–Cu alloys [J]. Materials Science and Engineering
A, 2015, 621: 173–181.
[8] WEN Kai, FAN Yun-qiang, WANG Guo-jun, JIN Long-bin,
LI Xi-wu, LI Zhi-hui, ZHANG Yong-gan, XIONG Bai-qing.
Aging behavior and precipitate characterization of a high
Zn-containing Al–Zn–Mg–Cu alloy with various tempers [J].
Materials & Design, 2016, 101: 16–23.
[9] FENG Lei, PAN Qing-lin, WEI Li-li, HUANG Zhi-qi, LIU
Zhi-ming. Through-thickness inhomogeneity of localized
corrosion in 7050-T7451 Al alloy thick plate [J]. Journal of
Central South University, 2015, 22(7): 2423–2434.
[10] ZHANG Zhi-ye, PAN Qing-lin, ZHOU Jian. Hot
deformation behavior and microstructure evolution of
Al–Zn–Mg–0.25Sc–Zr alloy during compression at elevated
temperatures [J]. Transaotions of Nonferrous Metals Society
of China, 2012, 22(7): 1556–1562.
[11] PEREZ M, DUMONT M, ACEVEDO-REYES D.
Implementation of classical nucleation and growth theories
for precipitation [J]. Acta Materialia, 2008, 56(9): 2119–
2132.
[12] ROKHLIN L L, DOBATKINA T V, BOCHVAR N R,
LYSOVA E V. Investigation of phase equilibria in alloys of
the Al–Zn–Mg–Cu–Zr–Sc system [J]. Journal of Alloys and
Compounds, 2004, 367(1, 2): 10–16.
J. Cent. South Univ. (2018) 25: 961–975
[13] SENKOV O N, SHAGIEV M R, SENKOVA S V,
MIRACLE D B. Precipitation of Al3(Sc,Zr) particles in an
Al–Zn–Mg–Cu–Sc–Zr alloy during conventional solution
heat treatment and its effect on tensile properties [J]. Acta
Materialia, 2008, 56(15): 3723–3738.
[14] YAN Jie, PAN Qing-lin, ZHANG Xiang-kai, SUN Xue, LI
An-de, ZHOU Xun. Characterization of hot deformation
behavior of Al–Zn–Mg–Mn–Zr alloy during compression at
elevated temperature [J]. Journal of Central South University,
2017, 24(3): 515–520.
[15] ROBSON J D, PRANGNELL P B. Dispersoid precipitation
and process modelling in zirconium containing commercial
aluminium alloys [J]. Acta Materialia, 2001, 49(4): 599–613.
[16] RIDDLE Y W, SANDERS T H. A study of coarsening,
recrystallization, and morphology of microstructure in
Al–Sc–(Zr)–(Mg) alloys [J]. Metallurgical and Materials
Transactions A: Physical Metallurgy and Materials Science,
2004, 35A(1): 341–350.
[17] HUANG Xing, PAN Qing-lin, LI Bo, LIU Zhi-ming,
HUANG Zhi-qi, YIN Zhi-min. Effect of minor Sc on
microstructure and mechanical properties of Al–Zn–Mg–Zr
alloy metal–inert gas welds [J]. Journal of Alloys and
Compounds, 2015, 629: 197–207.
[18] ZHAO Jun-wen, XU Chao, CAI Guang-ze, WU Shu-sen,
HAN Jing. Microstructure and properties of rheo-diecasting
wrought aluminum alloy with Sc additions [J]. Materials
Letters, 2016, 173: 22–25.
[19] OROWAN E. Theory of the fatigue of metals [J].
Proceedings of the Royal Society of London Series
A-Mathematical and Physical Sciences, 1939, 171(A994):
0079–0106.
[20] SARHAN A A D, ZALNEZHAD E, HAMDI M. The
influence of higher surface hardness on fretting fatigue life
of hard anodized aerospace AL7075-T6 alloy [J]. Materials
Science and Engineering A, 2013, 560: 377–387.
[21] LI Meng-jia, PAN Qing-lin, WANG Ying, SHI Yun-jia.
Fatigue crack growth behavior of Al–Mg–Sc alloy [J].
Materials Science and Engineering A, 2014, 598: 350–354.
[22] PARIS P C. The growth of cracks due to variations in load
[D]. Lehigh University, 1962.
[23] GUAN Ming-fei, YU Hao. Fatigue crack growth behaviors
in hot-rolled low carbon steels: A comparison between
ferrite–pearlite and ferrite–bainite microstructures [J].
Materials Science and Engineering A, 2013, 559: 875–881.
[24] HUTCHINSON C R, de GEUSER F, CHEN Y,
DESCHAMPS A. Quantitative measurements of dynamic
precipitation during fatigue of an Al–Zn–Mg–(Cu) alloy
using small-angle X-ray scattering [J]. Acta Materialia, 2014,
74: 96–109.
[25] HAN W Z, VINOGRADOV A, HUTCHINSON C R. On the
reversibility of dislocation slip during cyclic deformation of
Al alloys containing shear-resistant particles [J]. Acta
Materialia, 2011, 59(9): 3720–3736.
[26] WANG Yin-lin, PAN Qing-lin, WEI Li-li, LI Bo, WANG
Ying. Effect of retrogression and reaging treatment on the
microstructure and fatigue crack growth behavior of 7050
aluminum alloy thick plate [J]. Materials & Design, 2014, 55:
857–863.
[27] ZHAO Y L, TANG Z Q, ZHANG Z, SU G Y, MA X L.
J. Cent. South Univ. (2018) 25: 961–975
Double-peak age strengthening of cold-worked 2024
aluminum alloy [J]. Acta Materialia, 2013, 61(5):
1624–1638.
[28] WEI Li-li, PAN Qing-lin, HUANG Xing, FENG Lei, WANG
Ying. Influence of grain structure and crystallographic
orientation on fatigue crack propagation behavior of 7050
alloy thick plate [J]. International Journal of Fatigue, 2014,
66: 55–64.
[29] SHI Yun-jia, PAN Qing-lin, LI Meng-jia, HUANG Xing, LI
Bo. Effect of Sc and Zr additions on corrosion behaviour of
Al–Zn–Mg–Cu alloys [J]. Journal of Alloys and Compounds,
2014, 612: 42–50.
[30] LI Chen, PAN Qing-lin, SHI Yun-jia, WANG Ying, LI Bo.
Influence of aging temperature on corrosion behavior of
Al–Zn–Mg–Sc–Zr alloy [J]. Materials & Design, 2014, 55:
551–559.
[31] MARLAUD T, DESCHAMPS A, BLEY F, LEFEBVRE W,
BAROUX B. Evolution of precipitate microstructures during
the retrogression and re-ageing heat treatment of an
Al–Zn–Mg–Cu alloy [J]. Acta Materialia, 2010, 58(14):
4814–4826.
中文导读
热处理对 Al–Zn–Mg–Sc–Zr 合金的显微结构及疲劳裂纹扩展行为的影响
摘要：本文采用电子背散射衍射（EBSD）、透射电子显微分析（TEM） 、扫描电子显微分析（SEM）
室温拉伸性能测试和疲劳裂纹扩展测试的方法研究了 4 种时效处理（欠时效、峰时效、过时效和双级
时效）对 Al–Zn–Mg-Sc–Zr 合金的显微组织和疲劳裂纹扩展行为的影响。结果表明： 合金中的 Al3(Sc,Zr)
粒子能显著地细化合金晶粒、提升拉伸性能和抗疲劳裂纹扩展性能。其中，欠时效样品和双级时效样
品的平均晶粒尺寸分别为 4.9473 μm 和 4.1257 μm，峰时效处理后样品达到最高的屈服强度和抗拉强
度（561 MPa 和 581 MPa）。基于 Laird 模型和 Griffith 理论，本文研究了合金在 Paris 区域中的裂纹
扩展速率、裂纹曲折与分叉、裂纹钝化与裂纹的沿晶和穿晶扩展行为。结果表明，欠时效样品表现出
最佳的抗疲劳裂纹扩展性能，其裂纹路径最为曲折、裂纹分叉最多。在高速扩展区域中，所有样品的
疲劳裂纹扩展速率均和屈服强度负相关。
关键词：Al–Zn–Mg–Sc–Zr 合金；热处理；显微组织；疲劳裂纹扩展速率；疲劳裂纹扩展路径
975
[32] GUO Wei, YANG Meng, ZHENG Yi, ZHANG Xue-shu, LI
Hui, WEN Xi-yu, ZHANG Jing-wu. Influence of elastic
tensile stress on aging process in an Al–Zn–Mg–Cu alloy [J].
Materials Letters, 2013, 106: 14–17.
[33] LI Gen, ZHAO Nai-qin, LIU Tao, LI Jia-jun, HE Chun-nian,
SHI Chun-sheng, LIU En-zuo, SHA Jun-wei. Effect of Sc/Zr
ratio on the microstructure and mechanical properties of new
type of Al–Zn–Mg–Sc–Zr alloys [J]. Materials Science and
Engineering A, 2014, 617: 219–227.
[34] NIKULIN I, KIPELOVA A, MALOPHEYEV S,
KAIBYSHEV R. Effect of second phase particles on grain
refinement during equal-channel angular pressing of an
Al–Mg–Mn alloy [J]. Acta Materialia, 2012, 60(2): 487–497.
[35] CAVALIERE P, CABIBBO M. Effect of Sc and Zr additions
on the microstructure and fatigue properties of AA6106
produced by equal-channel-angular-pressing [J]. Materials
Characterization, 2008, 59(3): 197–203.
[36] LAIRD C, SMITH G C. Crack propagation in high stress
fatigue [J]. Philosophical Magazine, 1962, 7(77): 847–857.
(Edited by YANG Hua)
、