Materials Characterization
journal homepage: www.elsevier.com/locate/matchar
The eects of heat treatment on the microstructure and cyclic behavior of MARK
A7N01-T4 aluminum alloy
Yi Duana, Jijin Xua,, Jingyao Chena, Chun Yua, Junmei Chena, Hao Lua,b
a
School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, PR China
b
Shanghai Key Laboratory of Materials Laser Processing and Modication, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai
200240, PR China
A R T I C L E I N F O A B S T R A C T
Keywords: Multi-level tension-compression tests were carried out on A7N01-T4 samples undergoing a series of non-iso-
Cyclic hardening thermal heat treatments beforehand. Transmission Electron Microscopy (TEM) and Dierential Scanning
Secondary precipitation Calorimetry (DSC) were performed to analyze the evolution of precipitations. Thermal cycles have signicant
Non-isothermal cycle inuence on its plastic constitutive relation. In an interval of peak temperature from 350 C to 450 C, the alloy
Aluminum alloy
re-precipitates a large number of non-shearable and precipitates and mainly presents kinematic hardening
characteristic due to the anisotropy induced by Orowan Loop Helped Reverse Bypass (OHRB) mechanism.
Strengthening precipitates grow coarser below this interval and decompose into aluminum matrix over this
interval, which are in favor of the dislocation shearing and interaction, and lead to an isotropic hardening
behavior of the alloy.
1. Introduction toughness and the yield strength of AA7050 aluminum alloy, and found
that coarse intragranular precipitates played a key role in the decrease
7XXX series aluminum alloy, as a typical kind of age-hardening of the intrinsic toughness of the grain interiors. Hrnqvist and Karlsson
alloy, shows high strength, excellent formability, corrosion-resistance [4] tested an extruded AA7030 alloy in low-cycle fatigue undergoing
and good weldability as well as low density. Nowadays, A7N01 is one of heat treatment. It was been found that the fatigue life was longer in the
the most ideal structural materials for lightweight vehicles and its NA temper due to its promotion to transgranular cracking. However,
rolled plate on aging temper of T4 has been widely used in the manu- few eorts have been made to focus on the integral behaviors of mul-
facture of high-speed train. However, softening phenomenon of welding tilevel cyclic deformation of 7XXX aluminum alloy. Recently, Bardel
joints becomes the bottleneck of its further application in practice. The et al. [5] performed a series of cyclic loading tests on aluminum alloy
researches of Cvijovi et al. [1] and Chen et al. [2] pointed out that specimens undergoing dierent thermal cycles to integrate the re-
thermal processes inuenced the microstructure of age-hardening alu- lationship among heat treatment, strength and strain hardening. But the
minum alloy dramatically because of changing the dimension and vo- material tested was A6061-T6 alloy, whose mechanical performances
lume fraction of precipitates in matrix, and led to a comprehensive and phase evolution are very dierent from that of A7N01 alloy,
decline of mechanical properties. Among that, the strain hardening of especially for dierent initial temper. Hence, the eects of thermal
the aluminum alloy and its essential mechanism is a key issue to de- cycles on the microstructure and cyclic behavior of A7N01-T4 alu-
termine its plastic behaviors, especially for fatigue life. When working minum alloy needs more detailed researches.
load exceeds yield point, the alloy produces a certain amount of plastic In present study, non-isothermal heat treatments, representative of
deformation instead of destroying directly, and with the increase of thermal cycles on heat-aected zone (HAZ) of welding joint, were im-
cycle times the plastic deformation accumulates constantly and nally posed on dierent A7N01-T4 specimens to obtain specic welding
leads to a fracture failure. microstructures. Quantitative mechanical characterization was per-
Over the decades, the mechanical response of aluminum alloy to formed on these specimens with uniaxial cyclic tension-compression
thermal treatment during manufacturing processes such as welding has tests, and then semi-quantitative microstructure analysis were con-
drawn increasing attention. Dumont et al. [3] investigated the eect of ducted by Transmission Electron Microscopy (TEM), Selected Area
process parameters of heat treatment on the compromise between the Diraction (SAD) and Dierential Scanning Calorimetry (DSC). The
Corresponding author.
E-mail address: xujijin_1979@sjtu.edu.cn (J. Xu).
http://dx.doi.org/10.1016/j.matchar.2017.07.020
Received 5 May 2017; Received in revised form 22 June 2017; Accepted 5 July 2017
Available online 06 July 2017
1044-5803/ 2017 Elsevier Inc. All rights reserved.
Y. Duan et al. Materials Characterization 131 (2017) 201209
Table 1
Chemical compositions of A7N01 alloy (wt%).
Si Fe Cu Mn Mg Cr Zn Ti
2. Experimental Methods
The base material used in this study was commercial A7N01-T4 Fig. 2. Test process curves at peak temperature 500 C.
alloy in the form of a rolled plate of 22 mm thickness and its chemical
compositions were specied in Table 1. The fusion temperature of the and tri-level strain cycles was specied in Fig. 2.
alloy is about 635 C according to industrial production practice.
Standard Low Cyclic Fatigue (LCF) specimens were rstly machined
from the plate with their longest axis taken along rolling direction of 2.3. Microstructure Analysis
the plate, and then subjected to a serial of thermal cycles up to dierent
peak temperatures of 25 C, 200 C, 250 C, 300 C, 350 C, 400 C, Microstructural evolution of the specimens was investigated by
450 C, 500 C, 550 C, respectively. The heating process of each optical and thermodynamic methods. TEM and SAD observations were
thermal cycle was accomplished with an infrared furnace. The dimen- conducted on a JEOL-2100F microscope operating at 120 kV. The chips
sions of the furnace chamber are 60 mm 40 mm 80 mm. The were cut from the center of cross-section of 20 mm central part, and
heating rate was set to 15 C/s. During heat treatment, three thermo- thinned by jet polishing in an electrolyte of 10% perchloric acid and
couples were evenly placed along the 20 mm central part and touched 90% ethanol at the temperature of 25 C and the voltage of 30 V.
on the surface of specimen to control accurately thermal histories and The continuous process of precipitates evolution of base material
assure no temperature gradient along axial direction. Due to low throughout the heating range from 20 C to 550 C was investigated by
heating rate and high thermal conductivity, the temperature deviation DSC test to detect transient phase transformation or secondary pre-
between the surface and the center is less than 5 C based on numerical cipitation during heat treatment. The testing device was Germany 204-
simulation results, which can be regarded as uniform-temperature zone F1 thermal analyzer with a continuous heating rate of 80 C/min under
during heat treatment. Once preset peak temperature on surface was pure argon ow at a rate of 50 ml/min. The sample used for DSC test
reached, the furnace was immediately opened and conducted with was cut from the mechanical specimen at initial T4 state and machined
natural air-cooling. The heating device and specimen were shown in to a 3 mm 0.5 mm disc with a weight of 8.7 mg.
Fig. 1.
3. Results
2.2. Mechanical Characterization
3.1. Cyclic Deformation Behavior
Once above heated specimens cooled down, cyclic tension-com-
pression tests were immediately conducted on a computer controlled There are two kinds of widely acknowledged constitutive relations
MTS servo-hydraulic machine at room temperature to avoid natural of cyclic hardening in the eld of material mechanics [6]: isotropic
aging. During the test, tri-level strain cycles with increasing amplitudes hardening and kinematic hardening. The isotropic hardening means
of 0.5%, 1.0% and 1.5% were performed on a specimen at strain rate of that the yield surface changes uniformly in all directions such that the
5 10 4/s, in the way of repeating the same tension-compression yield stress increases (or decreases) in all stress directions as plastic
loading under identical amount of strain for 10 times. The strain was strain occurs, which can be described by Eq. (1) [7,8]:
measured by a particular MTS strain gauge and all mechanical tests
were duplicated twice. A typical test process including one heat cycle = M(k1 k2 ) (1)
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stage of cycling, except for 500 C and 550 C, which presents a typical
feature of kinematic hardening. But as the strain goes up to more than
1%, most curves like 25 C, 200 C and 500 C begin showing isotropic
hardening characteristics. The higher the temperature goes, the
stronger the isotropic hardening trend is, which is similar to Bardel's [5]
results. This phenomenon indicates that the limitation surface of
backstress exists and isotropic hardening component takes more and
more important role as deformation accumulates.
The separation of the kinematic and isotropic hardening compo-
nents is traditionally investigated using strain-reversal tests that enable
characterization of the Bauschinger eect [11], referring to a phe-
nomenon where yield stress of material changes with loading direction.
The internal stress < > , the half of dierence between the stress
value at maximum forward stress Fmax and the reverse yield stress
R0.02, is the most eective variation to evaluate Bauschinger eect.
However, internal stress indeed depends on the plastic strain oset. In
this work, the plastic strain oset is set at 0.02% [5]. For the con-
venience of comparison, the relative value of each internal stress < >
Fig. 3. Three-dimensional representation of the hardening in isotropic/kinematic model
was calculated by Eq. (3). It can accurately reect the kinematic com-
[10]. ponent of strain hardening while ignore the absolute value of initial
yield strength of samples. The process to obtain the internal stress has
where is dislocation density and is ow strain, k1, k2 and M are three steps: (i) The true stress vs. true strain curve was plotted; (ii) The
material related constants. compressive data was reversed and plotted as a function of cumulative
The kinematic hardening is often used to model the behavior of strain; (iii) The elastic strain was removed and the true stress vs. cu-
metals subjected to cyclic loading where yielding of the metals is in- mulative true strain was regarded as a monotonic behavior. An example
dependent of the equivalent pressure stress. The evolution of backstress of reverse cycles at 200 C are presented in Fig. 6.
is dened by Ziegler's hardening rule [9]: < > = (Fmax R0.02) 2Fmax (3)
pl C Fig. 7 shows the nal result of characterization as a function of peak
= C ( ) +
0 C (2) temperature. The overall evolution trend of kinematic hardening
component is similar to that of cyclic mechanical curves discussed
pl
where C is the hardening parameter, is the work-hardening slope of above. The higher the peak temperature is, the less the kinematic
0
the isothermal uniaxial stress-strain response and C is the rate of change hardening contributes, except for the breakpoint at 350 C. Another
of C with respect to time. The evolution law for the kinematic hard- interesting point is that the maximum value is no more than 50%,
ening component implies that the yield surface translates as the which means that the isotropic hardening component works on alloy's
backstress changes, while constraining within a cylinder of hardening throughout all heat treatments.
radius 2 3 s , where s is the magnitude of at saturation (large For cyclic deformation, another important mechanical performance
plastic strains). In result any stress point must lie within a cylinder of is its initial yield stress, which can be measured from the rst cycle of
radius 2 3 max since the yield surface remains bounded, schematized each test. Fig. 8 presents the evolution of yield stress as a function of
as Fig. 3. peak temperature reached during the thermal cycle. It shows that the
Fig. 4 is a set of cyclic stressstrain curves obtained directly from yield stress strongly dependent on the peak temperatures ranging from
practical tests. The curve at 550 C only validates to the beginning of 200 C to 450 C, which may relate to the equilibrium transformation of
third cyclic stage due to tensile fracture during test. It is easy to nd metastable phase. Outside this temperature interval, the variation of
that all curves show cyclic hardening features since the stress amplitude yield stress is small. The yield strength of 500 C specimen even exceeds
keeps increasing during test. In isotropic hardening relation, the alloy that of 450 C, which may be caused by re-precipitation of low-potential
strength increases in all directions so the stress increases constantly as phases like GP zone during natural cooling.
the plastic strain cumulates even in the same strain level of cycles,
which can be seen as the curves at 25 C, 200 C, 300 C, 500 C and 3.2. TEM and SAD Observation
550 C: Firstly, the obvious divergence of cyclic circles in same stage
makes the entire pattern look very disperse and thick; Secondly, the A complex and multi-scale precipitation sequence may occur during
stress amplitude crossing two dierent strain levels indicates a sig- heat treatment, especially for the base aluminum alloy used in this
nicant increase resulting in a much stronger hardening. Both features study, whose initial state is standard-T4 commercial temper. An over-
are typical behaviors of isotropic hardening. By contrast, the strength view of precipitation TEM associated with the peak temperatures is
increases along plastic deformation direction while decreases reversely shown in Fig. 9. It should be mentioned that just several representative
in kinematic hardening relation, so the amplitude is not changed under temperatures were selected to explain the microstructural evolution,
same strain level. For instance, the curves at 350 C, 400 C and 450 C, since it was very dicult to discern microstructural dierences only by
whose tendency are convergent and ultimate hardening amount is unaided viewing when two temperatures were close.
small. In the base material (peak temperature = 25 C), small dot-like and
In order to characterize the cyclic hardening behaviors at dierent cylindrical precipitates with a size of less than 50 nm distribute sparsely
peak temperatures in a more perceivable way, the maximum stress inside the lattice grain. Outside the viewing range of this image or in
amplitudes were measured within each cycle, and its relationship with other micrographs, some irregularly shaped precipitates with unusually
the peak temperatures was plotted in Fig. 5. From an overall perspec- sizes of more than 200 nm appear sometimes, which apparently have
tive, there are large dierences between low temperature and high little chance to be strengthening phases. According to additional SEM
temperature, and a signicant transformation of hardening behavior and EDS analysis on the surface of TEM samples they may be con-
happens at 350 C. Locally viewing, it can be noticed that maximum stituent dispersoids in form of Al10Cr3 or Al-Mn compounds. Similar
stress amplitudes under identical strain loads are identical at the initial constituent dispersoids get observed persistently in earlier literatures,
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phase also gets weakened. smallest. It also explains the coupling peak between 250 C and 350 C
on DSC curve. Away from 350 C, all the precipitates tend to coarsen
4. Discussion and their density declines when the peak temperatures of heat treat-
ment rise. However, the abnormal increase of precipitation density at
4.1. Inuence of Heat Treatment on Microstructure 300 C reveals that the beginning temperature of re-precipitation may
be earlier than 300 C.
The results presented above draw a clear picture of bi-level evolu-
tion of precipitate microstructures across the heat treatments: On the 4.2. Inuence of Heat Treatment on Cyclic Behavior
one hand, pre-precipitated phases undergo severe coarsening and par-
tial dissolution as peak temperature goes up; On the other hand, mas- In essence, the inuence of heat treatment on mechanical properties
sive new precipitates of strengthening phases heterogeneously re-pre- depends on the evolution of microstructure. From Figs. 7 and 12, the
cipitate from solution at intermediate temperature and undergo the relationship between precipitate density and hardening behaviors can
same process. To elucidate this evolution in a more quantitive way, the be gured out. The higher the precipitate density, the higher the ki-
mean size and density of precipitations on TEM micrographs were nematic hardening is. The more the precipitates get dissolved, the faster
measured and analyzed with the help of image software ImageJ. At the isotropic hardening accumulates. Traditionally, precipitation con-
least six random pictures of each specimen were examined to ensure the tribution on strain hardening can be assessed as Orowan Loops Me-
reliability of results. chanism (OLM), thanks to previous works of Ashby [21], and Brown
The statistic results shown in Fig. 12 prove the assumption again. and Stobbs [22]. However, this theory only considers unidirectional
Initial T4 material is a stable natural-aging state after full solution movement of dislocation and cannot explain why internal stress gen-
treatment. The precipitates presenting in this material are mainly tiny erates under cyclic loads. A possible interpretation is that, in line with
GP zones and phase with quite low density, which gets good reec- the initial suggestion by Gould [23], the encountering of gliding dis-
tion in TEM observation. Due to the pre-precipitation of GP zones, the locations with opposite Burgers vector brings about the annihilation of
insucient supersaturation of matrix solution reduces its potential Orowan loops stored around the non-shearable precipitates [6]. This
energy for phase nucleation and leads to a higher precipitation mechanism is illustrated as Fig. 13. During the last step of forward
temperature. When the elevated temperature of precipitation is equal strain, dislocations piled up at both sides of a non-shearable precipitate
to that of phase, an excessive driving force of combined phase A, with opposite Burgers vector (assuming the left are negative and the
transformation prompts a vigorous and multi-scaled precipitation in- right are positive), respectively. Dislocation 1 with negative Burgers
stantaneously. This phenomenon can be found at 350 C in Fig. 9, vector came over the plane of precipitate A somehow (e.g. cross slip-
where the precipitate density is extremely high but mean size is the ping from the plane of precipitate B). Once backward strain was loaded,
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Fig. 10. The SAD patterns and phase calibration of specimens. (a) at
25 C in [011]Al, (b) at 350 C in [001]Al, (c) at 350 C in [111]Al,
(d) at 550 C in [111]Al, (e) at 550 C in [011]Al.
Fig. 11. DSC curve of A7N01-T4 alloy. Fig. 12. Mean size and density evolution of precipitates versus reached temperature.
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(1) The initial state of base material decides the formation of micro-
structure evolution while the thermal cycles play an important role
on the tendency of the evolution. The entire process demonstrates
two parallel evolutions: the growth-decomposition of pre-pre-
cipitated phases and the nucleation-growth-decomposition of re-
precipitated phases.
(2) The overall performance of A7N01-T4 aluminum alloy under cyclic
loadings presents a signicant hardening trend. In the temperature
interval from 350 C to 450 C, the alloy mainly shows a kinematic
hardening characteristics, while away from this interval its cyclic
behavior tends to be isotropic. This phenomenon gets a reasonable
explanation by OHRB, dislocation shearing and interaction me-
chanisms.
Acknowledgments
References
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