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: [email protected]
962 J. Cent. South Univ. (2018) 25: 961–975

strength and toughness are in badly need. A number to describe the relation of fatigue crack growth rate
of researches about micro-alloying have been da/dN and applied stress intensity factor range ΔK
conducted to further enhance the mechanical in the second region [22]. Many models have been
performance of Al–Zn–Mg alloys. Among dozens proposed to illustrate the process in the Paris region
of micro-alloying elements, the combination of Sc such as the slip band extrusion intrusion model,
and Zr is considered to be one of the most effective dislocation blocking model and crack tip blunting
elements due to the fact that the coherent Al3(Sc,Zr) and resharping model. However, none of them can
precipitates can effectively inhibit grain growth and explain the fatigue behavior of precipitation
prevent the motion of dislocations [10, 11]. It has hardened aluminum alloys. It is generally agreed
been reported that Sc and Zr can also interact with that heat treatment has significant influence on the
aluminum separately to form Al3Sc and Al3Zr fatigue properties as different microstructures can
precipitations, but the Al3Zr precipitation always lead to different crack propagation behaviors [23].
exhibits disordered distribution for the segregation Various heat treatments have been extensively
of Zr during solidification, while the Al3Sc phase studied to explore the effect of heat treatment on
can disperse uniformly for its higher solubility fatigue behavior [19, 24–27]. As early as the 1930 s,
[12–15]. PEREZ et al [11] and ROBSON et al [15] OROWAN [19] reported that metastable
confirmed that the disordered distribution of Al3Zr precipitates in peak-aged aluminum alloys will turn
precipitates can be remedied by the faster to over-aging state even at room temperature during
nucleating Al3Sc precipitates by forming a finer and cyclic deformation, resulting in a degradation of
dispersive Al3(Sc,Zr) phase. RIDDLE et al [16] mechanical performance. Recently, in HAN’s
found that alloys containing both Sc and Zr show reports [25] and HUTCHINSON’s [24], profuse
even better recrystallization resistance than either dynamic precipitations of aluminum alloys were
addition of Sc or Zr. Moreover, Sc is more costly observed during the process of cyclic deformation
than Zr, which restricts the commercial application at room temperature. The volume fraction of GP
of Al–Sc alloys. Consequently, the combination of zone increased in the under-aged states, and it was
Sc and Zr is applied in this work. Numerous found that under-aged aluminum alloys exhibited
researches have concentrated on the precipitation longer fatigue life compared with the peak-aged
behavior of Al3(Sc,Zr) particles and their grain ones. WANG et al [26] revealed that retrogression
refining effect. The effect of varied amount of Sc and reaging treated Al–Zn–Mg–Cu alloy, benefiting
addition on microstructure and mechanical from its precipitates in the matrix and the narrower
properties of Al–Zn–Mg–Zr alloy has been studied PFZs, demonstrated better fatigue property than
in our previous work [17]. The result showed that T7451.
the optimal amount of Sc is 0.25% (wt%), which However, previously reported studies mainly
can obtain the finest grain size. ZHAO et al [18] focused on the fatigue performance of Al–Zn–Mg–
also indicated that the addition of Sc contributes Sc–Zr alloys under different heat treatments. The
considerably in enhancing tensile strength and present work performs a detailed analysis on crack
ductility, as Sc can influence the morphology of the propagation process from microscopic view. And
primary α-Al in the slurry. the effect of different annealing treatments on the
The fatigue failure is known to be one of the microstructure and fatigue crack growth behavior of
main destruction causing air crashes [19–21]. studied alloy is also thoroughly investigated. These
Unfortunately, the fatigue resistance of aluminum results may offer useful information for optimizing
alloys is usually poor. Therefore, the study on the heat treatment system for industrial applications,
fatigue properties of aluminum alloys is necessary. and will be necessary for establishing a crack
As a result, fatigue crack growth behavior and propagation mechanism for Al–Zn–Mg–Sc–Zr
fatigue life prediction became quite heated in recent alloys.
years. Fatigue crack growth rate, the most
commonly used indicator to characterize the fatigue 2 Experimental procedures
properties of alloys, can be described by the
da/dN–ΔK curve which can be divided into three 2.1 Material
regions and the Paris law has been widely accepted Base metal used in the experiment was
J. Cent. South Univ. (2018) 25: 961–975 963
Al–Zn–Mg–Sc–Zr alloy, which was cast via used in the tests. All the tests were conducted in air
metallurgy with pure Al, Zn, Mg metals and Al–Cu, at room temperature, with a stress ratio (Pmin=
Al–Mn, Al–Sc, Al–Zr master alloys into 260 mm× 1.4 kN, Pmax=14 kN, R=Pmin/Pmax) of 0.1 and a
150 mm×30 mm ingots. Table 1 shows its chemical sinusoidal loading which was applied at a frequency
composition. The specimens were taken from the of 10 Hz. The length of fatigue crack was measured
middle of the ingot and homogenized at 470 °C for by an optical microscope (±1 μm) attached on the
24 h. Then a hot rolling process was applied to fatigue machine. The following equation was used
5.7 mm (77% rolling reduction) at 470 °C, which to determine the stress intensity factor ΔK:
was followed by intermediate annealing at 420 °C P π π
for 1 h. Subsequently, the hot-rolled sheets were K  sec (1)
B 2w 2
cold-rolled to a thickness of 2.0 mm (65%
reduction). The cold-rolled sheets were subjected to where P is the load (in MPa); B and w are the
solid solution treatment at 470 °C for 1 h, followed thickness (in mm) and the width of the sample,
by water quenching, and then the specimens were respectively; α=2ɑ/w, and ɑ is the half-crack length
aged at 120 °C for 4 h (under-aged sample, (in mm).
designated as UA), 24 h (peak-aged sample,
designated as PA), 48 h (over-aged sample, 2.3 Microstructural analysis
designated as OA), and 120 °C for 6 h then 140 °C To characterize the microstructure of samples
for 20 h (double-aging, designated as DA), detailedly, the transmission electron microscopy
respectively. (TEM) was utilized. The tested thin foils were
prepared by twin-jet electro-polishing at 20 V in a
Table 1 Chemical composition of Al–Zn–Mg–Sc–Zr
solution consisting of 30% nitric acid and 70%
alloy (mass fraction, %) methanol (vol.%) at –25 °C and observed on a
TECNAI G2 F20 electron microscope, with an
Zn Mg Cu Mn Sc Zr Al
acceleration voltage of 200 kV.
5.40 2.00 0.35 0.30 0.25 0.10 Bal.
The fatigue fracture surfaces and crack
propagation paths were analyzed on FEI QUANTA-
2.2 Tensile and fatigue crack growth rate tests 200 and Helios scanning electron microscopy
The tensile tests were conducted on MTS-858 (SEM).
tester. Specimens were taken from the plates in the To explore the crystallographic relationships
longitudinal transverse direction according to between fatigue crack path and the subgrain
ASTM E647 standard. For each sample, three morphology and orientation, electron backscattered
tensile specimens were tested and the average value diffraction (EBSD) methods was implemented with
of the results was adopted to evaluate the strength an accelerating voltage of 20 kV.
and ductility of the sample.
Fatigue crack growth tests were carried out on 3 Results and discussion
a MTS-810 test machine using middle-tension (MT)
specimens according to ASTM E647 standard. 3.1 Microstructure characterization
Figure 1 shows the major dimensions of the sample As shown in Figure 2, orientation distribution

Figure 1 Geometry of MT specimen (dimensions in mm)

964 J. Cent. South Univ. (2018) 25: 961–975

of the grains with the crack were measured by annealing treatments in EBSD analysis (Figure 2).
EBSD analysis accessory. Different orientations of Therefore, the TEM observation was applied to
the grains are marked by different colors and the further explore the detail microstructure inside
EBSD inverse pole-figure (IPF) map superposed grains. It is widely accepted that the precipitation
with the grain boundary (GB) component of the sequence of Al–Zn–Mg–Cu series aluminum alloys
crack reveals the grain structure. The high angle is showed as followings: supersaturated solid
boundary (>15°) and low angle boundary solution (α)→GP zone→metastable η′→
(2°<θ<15°) are delineated by lines in different equilibrium η (MgZn2) [7, 29]. GP zone is atom
colors. The misorientation angle distribution and clustering zone which is coherent with α(Al) matrix.
grain size statistics are shown in Figure 3. The η′ phase is a metastable hexagonal phase and is
According to the results, the average misorientation semi-coherent with α (Al) matrix. The η phase is an
angles of the UA sample and DA sample are equilibrium phase and is non-coherent with α (Al)
27.709° and 27.336°, and the average grain sizes matrix. And Al3(Sc,Zr) precipitate, the most
are 4.9473 μm and 4.1257 μm, respectively. WANG important type of precipitates in this work, is
et al [26] and WEI et al [28] studied the mechanical coherent with α(Al) matrix [30–32]. These
properties and fatigue fracture behavior of Al3(Sc,Zr) precipitates, dispersing in the grains and
Al–5.67Zn–1.92Mg–1.89Cu alloy with different at the grain boundaries, can pin dislocations and
heat treatments, and its composition is close to that grain boundaries, resulting in better resistance of
of the alloy used in this work except the present mechanical properties[29].
alloy containing a small amount of Sc and Zr. The Figure 4 shows the TEM images of the
average grain size of Al–5.67Zn–1.92Mg–1.89Cu samples with different annealing treatments. For the
alloy after aging treatment was about 50 μm, nearly UA sample (Figures 4(a) and (b)), no obvious
13 times ours, which proves that the addition of Sc precipitates can be found in the grains, and the
resulted in a good recrystallization resistance. grain boundaries were continuous. The inset image
There is no significant change of structural and in Figure 4(b) is the SAED pattern of the UA
grain size between samples under different sample obtained by projecting along the [011] Al

Figure 2 EBSD observations of fatigue crack behavior in Paris region: (a) UA sample; (b) DA sample
J. Cent. South Univ. (2018) 25: 961–975 965

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 In order to investigate the evolution of these
have been indexed, and those spots marked by the particles during annealing treatment, two TEM
white arrows are derived from Al3(Sc, Zr) particles images were selected randomly to calculate the
with a Ll2 cubic crystal structure. For the PA sample, average size of Al3(Sc,Zr) particles for each sample.
a large quantity of precipitates distribute Results show that the average equivalent diameters
homogenously in the grains, and the precipitates in of Al3(Sc,Zr) particles are 29.1 nm for UA sample,
grain boundaries are more apparent and coarser as 28.9 nm for PA sample, 29.3 nm for OA sample,
shown in Figures 4(c) and (d). The precipitation and 29.4 nm for DA sample.
free zone (PFZ) can also be observed, and its small In conclusion, with the degree of aging
width indicates that it was just formed during this treatment increasing, the precipitates in the grains
process. As the sample was aged to OA and DA became more apparent, which illustrates that GP
states (Figures 4(e) and (f)), the precipitates in the zones gradually transferred into uniformly
grain grew lager and the η precipitates coarsened dispersed η′ phases and the η′ phase transferred into
and became completely discontinuous along the coarser η phase. The grain boundary also became
grain boundaries. Meanwhile, the precipitation free more and more discontinuous and the PFZ
zone (PFZ) broadened. Compared with DA sample, broadened. Meanwhile, the nucleation and growth
the precipitates inside the grains of OA sample are of GP zones and η′ phase became much more
more unevenly dispersed and the precipitates in apparent. The size of Al3(Sc,Zr) particles generally
grain boundaries are more discontinuous and remains unchanged with an averaged diameter of
coarser. Petal-shaped Al3(Sc,Zr) precipitates can be about 29 nm.
observed in all samples (Figure 4). Around the
particles, a large number of dislocations and 3.2 Mechanical properties
dislocation tangles were observed, which proves Table 2 shows the tensile properties of the
that Al3(Sc,Zr) precipitates can pin the dislocation. 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 Figure 5 Double logarithmic plots of da/dN against ΔK:
this work are 21 MPa and 56 MPa higher, (a) UA sample and PA sample; (b) PA sample and DA
respectively. This improved performance can be sample
attributed to the countless uniformly dispersed fine
Al3(Sc,Zr) precipitates in the grains, which can be The fatigue crack propagation resistance of DA
clearly observed in Figure 4. These Al3(Sc,Zr) sample is slightly higher than that of OA sample.
precipitates were not only uniformly dispersed but However, when ΔK>27 MPa·m1/2, the curve of DA
also coherent with the Al matrix, which enabled sample shows a typical curving shape and its crack
them to contribute to stabilizing the fine grained expanding speed increases more quickly. And the
microstructure and strengthen the alloys by pinning curve of DA sample exhibits a wider range of ΔK
the grain boundary and hindering the dislocation than the OA one.
motion [33]. To quantify fatigue properties of four samples
The fatigue crack growth rates da/dN vs and analyze them more accurately, data fitting of
applied stress intensity factor ranges ΔK of samples the Paris region is necessary. The Paris region is the
with different annealing treatments are compared. linear region in the double logarithmic plot of
In the double logarithmic plot of da/dN against ΔK da/dN against ΔK, which can be described by the
is shown in Figure 5, in which the da/dN–ΔK curve following equation:
can be divided into three regions, the threshold da
 C (K ) m (2)
region, the Paris region and the rupture region. dN
As Figure 5(a) shows, the UA sample where m is the Paris exponent and C is the Paris
possesses a wider range of ΔK than the PA state. constant. The values of these two constants (C and
And when ΔK<30 MPa·m1/2, the UA sample m) can be obtained by data fitting for the Paris
exhibits a higher resistance to fatigue crack region of the plot. The fitted lines are displayed in
propagation as compared with the PA sample. But Figure 6, and the calculated values along with the
when ΔK>30 MPa·m1/2, the fatigue crack grew more corresponding fracture cycle numbers are listed in
quickly in the UA sample than in the PA sample. Table 3. According to the results, the DA sample
Figure 5(b) illustrates that the curves of OA and DA has smaller C and m than the OA sample, which
samples are almost identical in the first two regions. 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 J. Cent. South Univ. (2018) 25: 961–975

crack present a trans-granular propagation mode. the Griffith equation:

For the DA sample, the crack still mainly presents a 1
trans-granular extension, but inter-granular cracks  2 E  2
c    (3)
can also be observed both in the master crack and  πa 
second cracks (marked by black ellipses), which where E is elastic modulus; γ is the surface energy
differs from the UA sample.
(per unit area) and a is the half-crack length.
In order to investigate the interaction of fatigue
According to the Griffith theory, the extension
crack with particles, SEM and EDS techniques are
stress at the crack tip would be increased when the
employed in the analysis of UA sample. As shown
fatigue crack tip encounters particles that can be
in Figure 8(a), the fatigue crack cut the impurity
broken easily. Once these particles are broken, the
particles and advanced into the alloy matrix, which
crack will propagate a longer distance than that in a
can be proved by the small fragments left in the
crack. However, branching crack observed in region without stress concentration (Figure 8(a)). In
Figure 8(b) can be attributed to the deflecting and other words, the easily broken particles reduced the
retarding effect by Al3(Sc,Zr) particles. critical stress, which results in a sensitive resistance
The impediment caused by particles is an to fatigue crack propagation.
important factor in fatigue crack growth behavior. Oppositely, when the crack tip encountered
The Griffith theory holds that a flaw will propagate particles that only can be bypassed, like the η phase
in a stressed material only when it brings about a and Al3(Sc,Zr) particle, it stagnated momentary and
reduction in elastic stored energy more than then bypasses these particles because the stress is
sufficient to meet the free energy requirements of insufficient to break the particles and propagate on
the newly formed fracture surfaces [21]. The critical (Figure 8(b)). Therefore, the crack propagation was
stress required to propagate the crack is given by hindered by such particles.

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: 961–975 971

3.4 Fatigue fractographic analysis and fluctuation of the ratios between striation width and
mechanism analysis crack propagation rate is reasonable, and the results
To validate the fatigue properties of the are in good agreement with the measured crack
samples further and explore their mechanism at the propagation rates (Figure 5) and the fitting results
micro level, fractographs of the Paris region and the (Table 3).
rupture region were investigated. Figure 9 displays Generally speaking, the fracture of metals is
the fractographs of samples in Paris region governed by localized deformation that leads to a
(ΔK=22.157 MPa·m1/2), and all of the fractures very poor macroscopic ductility and dimpled
show the typical characteristics of striations. The fracture surfaces [35]. Figure 10 shows the
average striation distance and the corresponding fractographs in rupture region of these four samples.
fatigue crack growth rate of each sample are shown The presence of countless dimples indicates that all
in Table 4. As is well known, every fatigue cycle samples had showed a good quality of ductility and
produces a fatigue striation in Paris region [34]. their main failure mode was ductile trans-granular
That is to say, the narrower the fatigue striation mode. Compared with UA sample, PA and OA
distance is, the slower the fatigue crack grows, samples (Figures 10(b) and (c)) have much smaller
which indicates a better resistance to fatigue and more intensive dimples due to prolonged
propagation. Besides, second cracks inside the grain annealing treatments, which is the evidence of
can be clearly observed in the UA sample (Figure higher strength. Additionally, their tear ridges are
9(a)), which grew perpendicular to the direction of more obvious. Notably, inter-granular failure along
the lead cracks. Second cracks can also be found in grain boundaries can be observed in OA sample
DA sample (marked by arrows in Figure 9(d)) occasionally (pointed out by red arrows), which
although it is along the grain boundary and slighter. may explain its higher fatigue crack propagation
In general, the distance of striation is strictly rate in rupture region. And finally, for the DA
proportional to the crack propagation rate, but in sample, its fracture surface possesses the largest
this work this strictly proportional relationship is dimples, which explains its better elongation. And
broken due to the presence of second cracks, which tear ridges on its fracture surface are even more
can increase the total crack path. Thus, the slight obvious compared with those of the others. For all

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
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: 961–975 973

in this study, results of fatigue crack growth rate in blunting as it can retard the propagation. Therefore,
rupture region conformed this point. The PA sample the DA sample possesses a wider Paris region
possesses a higher yield strength, which is despite of its lower yield strength.
responsible for the wider Paris region and lower However, compared with the DA sample, the
fatigue crack growth rate when ΔK>30 MPa·m1/2. OA sample with the same wide PFZ exhibits a
Similarly, compared with DA sample, the fatigue narrower Paris region. This can be explained by
crack growth rate of OA sample in rupture region is their microstructure differences as follows. For the
lower owing to its higher yield strength. DA sample, it was reported before that the large
The results of crack path in EBSD analysis size and stable GP zone will be formed after
(Figure 2) demonstrate that the trans-granular mode pre-aging treated at 120 °C [7]. Then, the η′ phase
is the main way of the crack propagation in Paris nucleates and grows at effective GP zone formed
region, so optimizing the microstructure inside the before during the final aging at 140 °C. Hence,
grains is an important method to improve the compared with those of the OA sample, the
fatigue properties of alloys. Numerous studies have precipitates inside the grains of DA sample are
showed that precipitation hardened aluminum more uniformly dispersed, which is the reason of its
alloys would experience profuse dynamic better fatigue properties. Moreover, the precipitates
precipitations inside the grains when they were at the grain boundary of OA sample are more
subjected to cyclic deformation due to the disordered and coarser than those of DA sample
instability of the precipitates’ microstructure [19, 24, (Figure 4), resulting in higher fatigue crack growth.
25]. Similarly, in this work, as the cyclic And this negative effect depleted the benefit
deformation goes, the metastable η′ phase formed in brought by the PFZ.
PA sample will gradually turn to over-aging state η
phase, whose strengthening effect is weaker than 4 Conclusions
the former one. While in the UA sample, the GP
zone formation is accelerated during the cyclic The effect of annealing treatment on the
deformation. Thus, the cyclic deformation will microstructure and fatigue crack growth behavior of
result in a degradation in the mechanical Al–Zn–Mg–Sc–Zr alloy has been investigated. The
performance for the PA sample and a promotion for following results can be concluded:
the UA sample. Moreover, crack branching and 1) During the aging treatments, the size of
deflection are also unneglectable factors. The Al3(Sc,Zr) particles keeps unchanged, maintaining
fractographs of crack paths and side views an average diameter of about 29 nm. And these
(Figure 7) illustrate that fatigue crack path in UA Al3(Sc,Zr) particles bring about a remarkable grain
sample is more tortuous and bifurcated, which can refining effect that for UA sample and DA sample
greatly reduce the fatigue crack growth rate. Based average grain sizes of 4.9 and 4.1 μm are obtained,
on the above points of view, the superiority of respectively. Besides, they also impede and deflect
fatigue properties of UA sample can be explained. the fatigue crack propagation by pinning up the
As shown in Figure 2(b), the wide PFZ dislocations, greatly improving the tensile
adjacent to the grain boundary in the DA sample properties and fatigue properties.
leads to its inter-granular crack propagation to some 2) Among these four samples, the UA sample
degree. There are two opposite theories about the exhibits the best fatigue properties, whose crack is
effect of PFZ on mechanical properties. One theory most bifurcated and deflects and propagates
believes that the PFZ is mechanically weaker than trans-granularly through the grains.
the matrix due to its depletion of solute. The other 3) Compared with the OA sample, DA sample
one holds that PFZ is so soft that it enhances the shows better fatigue properties, which can be
toughness. The results of the present work support attributed to its more uniformly dispersed
that the second one is more suitable for the current precipitates in the grains and more continuously
fatigue behavior considering the crack blunting. distributed finer precipitates at the grain boundaries.
Since the PFZ is almost equivalent to the pure This work also confirms that the wide PFZs in both
matrix, it is soft enough to relax the stress when the DA and OA samples are soft enough to release the
crack tip enters, and it is also beneficial to crack stress and arise crack blunting, resulting in
974 J. Cent. South Univ. (2018) 25: 961–975
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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