Materials Science and Engineering A
Materials Science and Engineering A
Materials Science and Engineering A
a r t i c l e i n f o a b s t r a c t
Article history: Magnesium, being the lightest available structural material, is a primary candidate for automotive and
Received 11 June 2008 aviation industries; however, the difficulty of deforming magnesium is a limiting factor. This research work
Received in revised form 12 October 2008 aims to investigate the deformability of AZ31 magnesium alloy employing various deformation conditions.
Accepted 16 October 2008
The results are used to correlate the effect of changing the deformation conditions on the resulting material
behavior and microstructure. Tensile testing experiments were conducted at a wide variety of deformation
Keywords:
conditions to determine the constitutive behavior of AZ31 magnesium alloy. The effect of changing the
AZ31 magnesium alloy
deformation conditions on the resulting microstructure is also examined and quantified by measuring the
Strain rate
Temperature
volume fraction and size of the dynamically recrystallized grains. Hardness measurements were employed
Dynamic recrystallization to determine the softening behavior of the material during deformation due to dynamic recrystallization.
Constitutive behavior The findings indicate a decrease in the peak stress and hardness and an increase in the fraction and size
Microstructure of dynamically recrystallized grains with decreasing strain rate and increasing deforming temperature.
Temperature plays a major role in determining the fraction and size of dynamically recrystallized grain
whereby, at a certain strain rate, an increase in temperature by 50 ◦ C results in a change in the fraction of
dynamically recrystallized grains by ∼30%. Further correlations were developed based on these findings
to optimize the deformation behavior.
© 2008 Elsevier B.V. All rights reserved.
0921-5093/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2008.10.033
I.A. Maksoud et al. / Materials Science and Engineering A 504 (2009) 40–48 41
−Q
2.1. Tensile testing
ε̇ = A exp(ˇ) exp (2)
RT
−Q The test conditions that were employed in this work are at tem-
ε̇ = A(sinh ˛)n exp (3) peratures ranging from 25 and 404 ◦ C and strain rates between
RT 1 × 10−4 and 1 × 10−2 s−1 . To ensure repeatability and accuracy,
each test condition was repeated at least three times. The tensile
where ε̇ is the strain rate, A , A , A, n , n, ˇ and ˛ are material
specimens were manufactured from extruded rods that according
constants, is the applied stress, Q is the activation energy for
to the DIN 50125 standard. It is worth mentioning that the extruded
deformation, R is the molar gas constant and T is the temperature.
rods were provided by Magnesium Elektron Co., UK as in kind sup-
In AZ31 magnesium alloy, Yi et al. [14] reported a decrease in
port.
the ultimate tensile stress at a strain rate of 5.5 × 10−4 s−1 from
Once fracture occurred, the specimens were quenched immedi-
307 to 70 MPa as the temperature increased from 25 to 250 ◦ C,
ately, in less than 5 s, in a water bath to prevent any microstructure
respectively, while Jäger et al. [15] reported a stress reduction at
change (static recrystallization or grain growth) [7]. For precise
1.3 × 10−4 s−1 from 343 to 14 to 7 MPa as the temperature increased
temperature measurement, one sample was manufactured with a
from 25 to 350 to 400 ◦ C, respectively. The mechanical testing
hole in the middle and the specimen temperature was measured
experiments carried out in AZ31 magnesium alloys [2,5,7,8,11,16]
using a type K thermocouple placed in this hole. Relations were
show a decrease in the material strength and an increase in the
developed, subsequently, to correlate the measured furnace tem-
ductility at elevated temperatures and low-strain rates. Guo et al.
perature to the sample actual temperature and were subsequently
[2] had also studied the effect of deformation conditions on the
used in this research.
peak stress of AZ31 magnesium alloy using compression tests and
reported that dynamic recrystallization (DRX) is the responsible
2.2. Metallography examination
mechanism for decreasing the peak stress at high temperatures and
low-strain rates. Other research work had also emphasized the role
After the specimens were quenched in a water bath, a longitu-
of DRX, the decrease of critical resolved shear stress (CRSS) for non
dinal sample, away by 2 cm from the neck, was cut. The samples
basal slip systems, which in turn activate these systems, and dislo-
were mounted, ground, polished and etched (3 g malic acid, 95 ml
cations annihilation on the reduction of the mechanical strength at
distilled water and 2 ml nitric acid). Optical microscopy examina-
high temperatures and low-strain rates [5,14,17].
tion was carried out using Zeiss Axio Imager Polarizer Microscopy
Barnett [11] established an Arrhenius function to account for
where at least eight micrographs were captured for each sample.
the constitutive behavior of AZ31 magnesium alloy with strain rate
sensitivity and activation energy of 0.15 and 145 kJ mol−1 , respec-
2.3. Hardness measurements
tively. Recently, Beer et al. [17] examined the microstructure of
compressed AZ31 magnesium alloy, at a temperature of 350 ◦ C and
Hardness measurements were conducting using Buehler
a strain rate of 0.01 s−1 , by studying the percentage and size of DRX
Micromet 2104 machine, hardness tests were conducted to the
grains at a strain up to 100% for wrought and cast AZ31 magnesium
mounted samples applying a load of 100 g. Hardness tests were
alloy and reported that the wrought material achieve 100% fraction
employed at least five times for each sample and the average was
of DRX grains and approximately 11 m DRX grain size as the strain
then calculated.
reaches 100%.
It is worth mentioning that the constants used to determine the
constitutive behavior relation, and the volume fraction and size of 3. Results
DRX grains based on tensile tests are rarely found in literature. The
quantification of the effect of deformation conditions, employing 3.1. Tensile testing
tensile testing conditions, on the resulting change in peak stress
and DRX grains has not been reported previously in literature. Fig. 1 shows the engineering stress strain curve of two extreme
This paper summarizes the findings of the research conducted to conditions (highest strain rate and lowest temperature versus low-
understand the workability and deformability of AZ31 magnesium
alloy. Extensive tensile experiments were carried out to under-
stand the constitutive behavior at various ranges of deformation
conditions, namely: temperature and stain rate and determine the
effect of changing these conditions on the resulting microstructure
and the material hardness. Based on these results, various relations
were developed to understand the effect of changing the deforma-
tion conditions on the deformability of AZ31 magnesium alloy.
2. Experimental work
Fig. 2. Effect of temperature on the peak stress of AZ31 magnesium alloy. Fig. 3. Effect of strain rate on the peak stress of AZ31 magnesium alloy.
Table 1
The relationship between temperature and percentage reduction in peak stress.
peak Pct. reduction (%) peak Pct. reduction (%) peak Pct. reduction (%)
Fig. 4. Optical microstructure of AZ31 magnesium alloy before deformation. Fig. 6. Optical microstructure of AZ31 magnesium alloy at T = 25 ◦ C and ε̇ = 1 ×
10−3 s−1 .
A comparison between Figs. 7 and 8 shows the strain rate also 4. Discussions and analysis
affect the fraction of DRX grains. As the strain rate increases, the
fraction of DRX grains decreases. In Fig. 9, the DRX grains could 4.1. Constitutive behavior of AZ31 magnesium alloy
be clearly observed as fine and equiaxed areas. By comparing
Figs. 7 and 9, it can be seen that as the temperature increases, The need for constitutive equations is to be able to quantify
the fraction of DRX grains also increases. It should be noted that the AZ31 magnesium alloy behavior at different deformation con-
at 213 ◦ C, the effect of dynamic recrystallization could not be ditions, temperatures and strain rates, in order to optimize its
observed. deformability. Eqs. (1) and (3) are the main relations used to
Fig. 5. Optical microstructure of AZ31 magnesium alloy at T = 25 ◦ C and ε̇ = 1 × Fig. 7. Optical microstructure of AZ31 magnesium alloy at T = 263 ◦ C and ε̇ = 1 ×
10−2 s−1 . 10−2 s−1 .
44 I.A. Maksoud et al. / Materials Science and Engineering A 504 (2009) 40–48
Fig. 10. Relation between logarithms of peak stress and strain rate (Eq. (4)).
tal measurements. This was proved by Barnett [11] where Eq. (1)
can only be used for peak stress values between 20 and 90 MPa.
To emphasize Barnett [11] findings, both equations are discussed
showing their average percentage error.
Fig. 8. Optical microstructure of AZ31 magnesium alloy at T = 263 ◦ C and ε̇ = 1 ×
10−4 s−1 .
4.1.1. Arrhenius equation
determining the constitutive behavior of AZ31 magnesium alloy 4.1.1.1. Stress exponent (n ). After some mathematical manipula-
[2,11–13,19,21,22]. Both equations do not depend on microstructure tions of Eq. (1), Eq. (4) was derived:
parameters such as initial grain size making them more applicable
1 ∂ log
in industrial fields since the maximum stress, required for defor- = (4)
n ∂ log ε̇
mation, is a function of deformation conditions (T, ε̇), material T
properties (Q, n) and one constant (A) only. By calculating the reciprocal of the slope of each linearly fitted
Although Eq. (1) can be easily applied in comparison to Eq. (3), line in Fig 10, the n value was calculated at each deformation condi-
the reported stress is not as accurate in comparison to experimen- tion. As can be seen from Fig. 10, the stress exponent is independent
at room temperature values so these data were excluded from the
sequence of obtaining n . The average n value was subsequently
calculated. As can be noted in Fig. 10, the slope of the linearly fit-
ted line changes with increasing temperature which could be an
indication of the change in the deformation mechanism [23].
The value of the stress exponent presented in this work is 7
which agrees with the findings of Barnett [11], which is approxi-
mately 7 but is higher than the findings of Huang et al. [12] which
is 5.3. However, it was reported that high-stress exponent values
could be due to the presence of fine oxides in the specimens [2].
Based on literature findings, it was found that a stress exponent
with the value of 7 is a climb controlled deformation mode [9,23].
This agrees with the findings of Ishikawa et al. [9] and also it is
common to have climb controlled deformation mode at elevated
temperatures [11].
where Z is the Zener–Hollomon parameter combining the effect of Measured stress − Predicted stress
Error (%) = × 100 (11)
strain rate and temperature shown in Eq. (7): Measured stress
Q
1
18
Z = ε̇ exp (7) Average error (%) = |Error (%)| (12)
RT 18
i=1
By calculating the y-intercept of each linearly fitted line in
Fig. 12, obtaining average values and calculating the exponential Barnett [11] reported that the Arrhenius equation is suitable only
of the average, the A values were calculated. in the stress range between 20–90 MPa but in this work, it is suitable
The A values proved to vary dramatically with changing the for stresses between 24 and 107 MPa and within 263 and 361 ◦ C.
temperature. However, the Arrhenius equation exhibits further The average percentage error is equal to 12%. The hyperbolic sine
sensitivity to the exponent parameters (Q, T) rather than the pre- function shows an average error less than 7%.
exponential constant (A ).
4.2. Microstructure evolution
Fig. 13. Effect of temperature on the volume fraction of dynamically recrystallized Fig. 15. Effect of temperature on dynamically recrystallized grain diameter of AZ31
grains of AZ31 magnesium alloy. magnesium alloy.
Fig. 14. Effect of strain rate on the volume fraction of dynamically recrystallized Fig. 16. Effect of strain rate on dynamically recrystallized grain diameter of AZ31
grains of AZ31 magnesium alloy. magnesium alloy.
on temperature, while the strain rate does not affect the fraction of for grain growth at higher temperatures. At lower strain rates, there
DRX grains significantly. is more time for the nucleation and growth events. Several research
work found also the same phenomena [9,10,17]. By comparing the
4.2.2. DRX grain size differences between the curves in Figs. 15 and 16, it can be seen
To determine the DRX grain diameter, the ASTM standard E112- that the temperature plays an important role than the strain rate in
96 was used. From Figs. 15 and 16, it can be seen that increasing affecting the DRX grain size.
the temperature and decreasing the strain rate increases the size of Analogous to the quantifications done on the percentage reduc-
DRX grains. This was expected since there is a higher driving force tion in the peak stress and percentage gain in the DRX volume
Table 2
The relationship between temperature and percentage gain in volume fraction of dynamically recrystallized grains.
Fraction rex. Pct. gain (%) Fraction rex. Pct. gain (%) Fraction rex. Pct. gain (%)
Table 3
The relationship between temperature and percentage gain in dynamically recrystallized grain size.
Drex (m) Pct. gain (%) Drex (m) Pct. gain (%) Drex (m) Pct. gain (%)
DRXdiameter = AZ −n (13)
Fig. 18. Average hardness at various temperatures.
4.3. Hardness
It was found that the hardness measurements are not sensi- 4.4. Operation and correlation curves
tive to the changes in the strain rate. It was also noted that as the
temperature increases, the hardness of the material decreases as Several correlations between the percentage reduction of peak
shown in Fig. 18. The decrease in hardness decreases with increas- stress and percentage gain of fraction and size of recrystallized
ing temperature could be attributed to the high fraction of DRX grains can be seen in Figs. 19 and 20. It can be noted in Fig. 19
grains. For example and as can be seen from Fig. 18, as the temper- that at a strain rate of 1 × 10−3 s−1 , the percentage gain of the vol-
ature increased from 213 to 321 ◦ C, the hardness values decreased ume fraction and diameter of DRX grains is almost equivalent as
from to 85 to 81 Hv . the temperature changes. Fig. 20 is a summary of various tables
presented in this paper to quantify the effect of changing the defor-
mation parameters on the percentage change in the peak stress
Fig. 17. Effect of temperature on dynamically recrystallized grain diameter of AZ31 Fig. 19. Correlations between size and the fraction of dynamically recrystallized
magnesium alloy. grains at 1 × 10−3 s−1 .
48 I.A. Maksoud et al. / Materials Science and Engineering A 504 (2009) 40–48