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Mg–14Li–1Zn Alloys www.aem-journal.com

Effects of Cold Rolling on Microstructural Evolution and

Mechanical Properties of Mg–14Li–1Zn Alloy
Kunning Fu, Jiahao Wang, Min Qiu, Fan Gao, Ruizhi Wu,* Legan Hou,
Haipeng Zheng, Jinhuai Zhang, and Milin Zhang

Zinc (Zn) is one of the main alloying

Cold rolling is employed to improve mechanical properties of Mg–14Li–1Zn elements in Mg–Li based alloy. The
alloy. Microstructural evolution and mechanical properties are investigated. addition of Zn can increase elongation
Results show that, as-cast and as-homogenized Mg–14Li–1Zn alloy is mainly obviously, but its strengthening effect is
low. The elongation of as-extruded Mg–
composed of β phase with trace amount of tiny α phase particles. During
8Li–1Zn alloy reaches 44%, about twice as
tensile test, the discontinuous α phase leads to intergranular fracture, which Mg–8Li–1Al alloy. However, the strength of
is a main reason for the low strength and low elongation. After cold rolling, Mg–8Li–1Zn is less than that of Mg–8Li–
the distribution of α phase becomes much more dispersive. The tensile 1Al.[12–15] Due to the good plasticity, Mg–
fractural morphology changes from brittle intergranular fracture to dimple Li–Zn alloy can be easily cold-rolled with a
large reduction causing the improvement
fracture. The sheet with 70% thickness reduction possesses the ultimate
of mechanical properties.[16,17]
tensile strength of 212 MPa, elongation of 9.4%, and microhardness of As a kind of high Li content Mg–Li alloy,
60.12 HV. When the total rolling reduction is 90%, the tensile strength Mg–14Li alloy possesses a low density, and
decreases slowly to 210 MPa, but the elongation increases sharply to 19.8%. is adapt to plastic forming. These advan-
Strengthening mechanisms of the Mg–14Li–1Zn alloy are attributed to strain tages make it be very prospective for
hardening and grain refinement. Strain hardening plays an important role in applications in the fields of aerospace.
However, its low strength is the key
the enhancement of strength. Grain refinement and the appropriate distribu-
obstacle for its wide applications.[18]
tion of the α(Mg) can obviously improve the plasticity. In order to improve the mechanical
properties of Mg–14Li–1Zn alloy, Mg–
14Li–1Zn sheet was prepared by cold
rolling. Microstructural evolution and me-
1. Introduction chanical properties of Mg–14Li–1Zn alloy during cold rolling
were investigated. The deformation mechanism and grain
Magnesium (Mg) alloy is the lightest metal among the refinement mechanism were discussed.
engineering metallic materials. It possesses the advantages of
high specific strength and stiffness, good damping capacity, and
high-energy particle penetration resistance.[1–7] The applications 2. Experimental Section
of magnesium alloy bring about significant benefits in the aspect
of energy conservation and emissions reduction.[8,9] The density The materials used in experiments were pure magnesium
of Mg–Li alloys decreases due to the addition of lithium (Li). (99.99 wt%), pure lithium (99.99 wt%), and pure zinc
When lithium content is larger than 10.3 wt%, the microstruc- (99.90 wt%). The materials were melted in a graphite crucible
ture changes from α hexagonal-close-packed (hcp) þ β body- in a vacuum induction furnace. Before the heating process to
center-cubic (bcc) to β (bcc), which improves the plasticity 690–720  С, the furnace was pumped to vacuum and then was
obviously.[10,11,24,25] charged with pure argon. Then, the melt was poured into a
permanent mold under argon protection to obtain book-shape
ingots with the dimensions of 230  145  40 mm3. The actual
Prof. R. Z. Wu, Prof. K. N. Ning, J. H. Wang, L. G. Hou, compositions of Mg–14Li–1Zn alloys were measured by
Dr. H. P. Zheng, Dr. J. H. Zhang, M. L. Zhang inductively coupled plasma atomic emission spectrometry
Key Laboratory of Superlight Materials & Surface Technology (Ministry (ICP, JY Ultima2), as listed in Table 1.
of Education)
Harbin Engineering University The heat treatment process was conducted in a resistance
Harbin 150001, P. R. China furnace under neutral atmosphere. The as-cast ingot was
E-mail: ruizhiwu2006@yahoo.com homogenized at 200  С for 12 h and cut into plates with a
Dr. M. Qiu, F. Gao, Prof. R. Z. Wu thickness of 3–20 mm. Then the plates were rolled to 2 mm at
Key College of Science room temperature with a rolling reduction of 30%, 50%, 70%,
Heihe University and 90%, respectively. The reduction per pass was 15–20%.
Heihe 164300, P. R. China
The specimens for microstructure observation were polished
DOI: 10.1002/adem.201801344 by abrasive paper and etched with a solution of 3 vol% natal. The

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Table 1. Actual compositions of Mg–14Li–1Zn alloy, wt%. The hardness values of the specimens were measured with a
microhardness tester. The loading force is 100 gf, and the
Alloy Li Zn Mg holding time is 15 s. The tensile tests were carried out with an
Mg–14Li–1Zn 15.21 0.961 Bal. initial strain rate of 1  103 s1 at room temperature. The
dimensions of specimen for tensile testing were shown in
Figure 1. All the test values were obtained from the average of
three measurements.

3. Results and Discussions

3.1. Microstructure

Figure 2 shows the microstructure of the as-homogenized

Mg–14Li–1Zn alloy. The matrix of the alloy is β(Li) phase (bcc).
Some spherical phases distribute at the grain boundary of β(Li).
Combining the results of EDS, XRD and selected area diffraction
(SAD) for the spherical phase, it can be concluded that the
spherical phase is α(Mg) phase. It should be noted that, unlike
the α(Mg) phase in Mg-Li alloys in the previous literature,[19,25]
Figure 1. Dimensions of the tensile specimen (units: mm).
the α(Mg) phase in this work is not a hcp structure, but a bcc
structure whose PDF card number is 65-7219#. Why does the
extraordinary α(Mg) phase exist in Mg–14Li–1Zn? It still
microstructures were analyzed using the optical microscopy remains unclear. This will become our focusing research in
(OM) and scanning electron microscopy (SEM), compositions of the near future.
individual phases of the alloys were examined with the attached Figure 3 shows optical microstructure of the as-cast Mg–14Li–
energy dispersive spectroscopy (EDS). The distribution of 1Zn alloy and cold-rolled Mg–14Li–1Zn alloys with reductions of
dislocation, sub-grain and second phase were observed by 30%, 50%, 70%, and 90%. Grains of the as-cast alloy are
transmission electron microscopy (TEM). The phases of the inhomogeneous and coarse with an average grain size of
alloys were analyzed by X-ray diffraction (XRD) with Cu radiation 300–800 mm. When the rolling reduction is 30%, the grains near
at a scan rate of 5 min1 and a step size of 0.02 . the surface of the sheet have obvious plastic deformation, as

Figure 2. Microstructures of as-homogenized Mg–14Li–1Zn alloy. a) SEM microstructure with the spherical-like particles; b) EDS patterns for the
spherical-like particles; c) XRD patterns of as-homogenized Mg–14Li–1Zn alloy; d) TEM microstructure for the spherical phase and its SAD pattern.

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Figure 3. Optical microstructure of as-cast Mg–14Li–1Zn alloy and as-rolled Mg–14Li–1Zn alloy with different reductions. a) as-cast, b) 30%, c) 50%,
d) 70%, e) 90%.

shown in Figure 3b. There exist some slip bands, which are the alloy with 30% rolling reduction, lots of dislocations are
located at the direction of 45 to rolling direction (RD). More slip apparent in the distorted grains and there is almost no twins in
bands appear with the deformation increase, as shown in the grains, which differs greatly from the general deformation
Figure 3c. When the rolling reduction increases to 70%, as mechanism of Mg alloys. It is well known that Mg possesses a
shown in Figure 3d, a large amount of curved slip bands appear hcp structure. The homogeneous plastic deformation of Mg is
and the grains are no longer discernable. Dynamic recrystalliza- always accompanied with twinning, even at elevated tempera-
tion grains appear near the surface of the sheet, as shown in the ture.[20,21,26] However, the deformation mechanism of Mg–14Li–
inserted enlarged image. The average size of the grain is 1Zn alloy may be different from conventional Mg due to the
7.8  3.1 mm. When the total cold rolling reduction is 90%, as matrix structure of bcc. Meanwhile, a lot of dislocations pile up at
shown in Figure 3e, the grain boundaries become blurred, grain boundary, dynamic recovery occurs subsequently. The sub-
showing a significant uniform fibrous structure along the rolling grains are embedded among dislocations generated during the
direction. Dynamic recrystallization occurs in more and more cold rolling. The size of sub-grain is about 500 nm.
regions. The quantity of dynamic recrystallization grains The dislocation density and the number of sub-grain increase
obviously increases. At the same time, the distribution of α with the rolling reduction increasing to 50%, as shown in
phase becomes much more dispersive, which can be observed Figure 4c and d. When rolling reduction increases from 50% to
in the inserted enlarged image. Therefore, rolling with large 70%, dislocation density continuously increases. At the same
deformation contributes to the occurrence of dynamic time, there exist twins in the alloy. It can be seen that, with
recrystallization. the increase of rolling reduction, the equiaxed grains are crushed
Figure 4 depicts TEM microstructure of Mg–14Li–1Zn alloy into fragmentary grains, in which there are twins
after cold-rolling with reductions of 30%, 50%, 70%, and 90%. In and dislocations. The results indicate that a large amount of

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dislocation wall, which in turn forms a sub-grain.

In the other word, when the total cold rolling
reduction is 90%, the dislocation density reduces
rapidly and the number of sub-grains increases
rapidly.

3.2. Mechanical Properties

Figure 5 shows the microhardness of as-cast Mg–

14Li–1Zn alloy and as-rolled Mg–14Li–1Zn alloy with
different rolling reductions. Microhardness of the as-
cast Mg–14Li–1Zn alloy is 41.02 HV. After cold rolling
with different reductions, due to strain-hardening, the
microhardness of Mg–14Li–1Zn alloy increases
greatly. When the cold rolling reduction is 70%, the
microhardness reaches the highest value, 60.12 HV.
When the total cold rolling reduction is larger than
90%, the microhardness decreases. It can be
explained that dynamic recrystallization occurs in
the alloy during the cold rolling deformation and the
dislocation density is reduced. The results show that,
when the rolling reduction is over 90%, work
softening occurs.
Figure 6 shows the stress-strain curves of the
samples. The tensile strength (UTS), yield strength
(YS), and elongation (EL) of the samples are listed in
Table 2. The tensile strength increases from 117 to
175 MPa after cold rolling with 30% rolling reduction.
The elongation almost does not change. During
subsequent cold rolling deformation, the tensile
strength and elongation increase with the increase
of rolling deformation. According to Figure 4a, the
hardening can be attributed to the lots of disloca-
tions.[19] When the rolling reduction increases to 70%,
the maximum tensile strength, 212 MPa, is obtained.
The twin boundaries act as strong obstacles to the
dislocation, leading to the high strain-hardening.
When the total rolling reduction is 90%, because the
dynamic recrystallization occurs and strain-hardening
reduces in the alloy, the tensile strength decreases to
210 MPa, but the elongation increases sharply to
19.8%.
When the total rolling reduction is less than 70%
including as-cast state, prior to the peak stress, the
stress increases with increasing strain. It indicates
that strain-hardening occurs in the specimens. When
the rolling reduction is 90%, strain-softening occurs,
dynamic recovery and local recrystallization is the
main softening mechanism. The specimen does not
fracture immediately after the stress attains the peak
Figure 4. TEM images of Mg–14Li–1Zn alloy with different rolling reductions. value. The plastic deformation sustains with a
a), b) 30%; c), d) 50%; e), f) 70%; and g), h) 90%. reduced stress. With the amount of grain boundary
increasing, the ability of resistance to deformation
improves. The cold-rolled alloy exhibits higher
sub-grains and the deformation twins form in the Mg–14Li–1Zn ductility as comparison with the as-cast alloy. The trend of
alloy with 90% rolling reductions. At the same time a lot of change in tensile test is slightly different from that of
paralleled dislocation walls emerge around the sub-grains. This microhardness test, which can be mainly attributed to the
indicates that the dislocations are rearranged to form a different strengthening mechanisms between them. During the

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Figure 5. Hardness of as-cast and as-rolled Mg–14Li–1Zn alloy with

different rolling reductions. Figure 6. Stress–strain curves of as-cast Mg–14Li–1Zn alloy and as-rolled
Mg–14Li–1Zn alloy with different rolling reductions.

microhardness test, the matrix locally undergoes plastic same time, densely populated micro-voids and dimples signify a
deformation, and the tensile test is the deformation of the ductile fracture. The numerous dimples and micro-voids are
sample as a whole. After dynamic recovery and local recrystalli- formed at the sites of precipitates during the tensile test.
zation, refinement strengthening becomes the main strength- Normally, ductile fractures are initiated by the soft β phase. This
ening mechanism. Obtaining the same stress concentration is consistent with the previous research.[22] Besides, Song
during the tensile test need to increase flow stress. Therefore, the et al.[23] reported that the fine α phase impedes dislocation
refinement strengthening improves the ultimate tensile movement causing the formation of microcrack because of the
strength. However, as for the microhardness, the locally non-homogenous deformation. The microcrack is beneficial to
undergone area covers only one or several grains. Therefore, the formation of dimples. Apparently, during cold rolling, the
the refinement strengthening effect is limited. tensile fracture morphology changes from brittle intergranular
fracture to dimple fracture. The strength and ductility of the alloy
both increase accordingly.
3.3. Fracture Microstructure The large fraction of dimples in Figure 7d indicates a good
ductility of the alloy with 70% rolling reduction. It should
From Figure 7a, it can be found that, there exist obvious cracks in be noted that, some cleavage planes can also be observed in the
the fracture microstructure and the fractural mode is intergran- inserted enlarged image. The size of the dimples in fracture
ular fracture. In the as-cast specimen, some α particles exist at surface of the alloy with 70% rolling reduction is similar to that
grain boundaries, and the grain boundaries are somewhat of the alloy with 50% rolling reduction, as shown in Figure 7c.
weaker than the inner grains. Crack forms along the grain Combining the results of the microstructure and stress-strain
boundary easily under the stress. Discontinuous precipitates at curves, the following conclusions can be drawn. The grains are
grain boundary can lead to intergranular fracture. This boosts broken during cold rolling. The dislocations pile up causing
the initiation of intergranular fracture. Crack propagation occurs serious strain-hardening. Therefore, the high strength can be
along grain boundaries that are embrittled by the induced obtained.
particles. The fractural characterization of the alloy with 30% In the alloy with 90% rolling reduction, a larger number of
rolling reduction in Figure 7b shows dual characteristics of dimples distribute throughout the fractography, as shown in
intergranular fracture and ductile fracture. The uneven
distribution of the stress and strain during the deformation
leads to uneven deformation of grains. On one hand,
pronounced ductile fractures are attributed to the refining Table 2. Mechanical properties of as-cast Mg–14Li–1Zn alloy and
effect caused by cold rolling. On the other hand, the as-rolled Mg–14Li–1Zn alloy with different rolling reductions.
discontinuous precipitates lead to the intergranular fracture,
as shown in the inserted enlarged image. UTS/MPa YS/MPa EL/%

Figure 7c consists of dual mixtures of brittle and ductile As-cast 117  2.2 98  3.1 3.1  0.1
fractures. Remarkably, as shown in the inserted enlarged image, 30% 175  3.1 153  3.3 3.3  0.1
propagated cleavage fractures initiated within the grains get 50% 193  2.6 180  2.9 5.3  0.2
arrested at the grain boundaries. The grain boundaries can
70% 212  3.5 192  3.2 9.4  0.2
hinder the initiation and extension of cracks, which further
90% 210  3.4 196  2.1 19.8  0.4
verifies the refinement strengthening in Mg–14Li–Zn. At the

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Figure 7. Tensile fracture morphologies of as-cast Mg–14Li–1Zn alloy and as-rolled Mg–14Li–1Zn alloy with different rolling reductions. a) as-cast,
b) 30%, c) 50%, d) 70%, e) 90%.

Figure 7e. The area fraction and size of dimples determine the Discontinuous α phase leads to intergranular fracture, which is
ductility of the alloys. It is obvious that the area fraction a main reason for the low strength and low elongation.
of dimples in the inserted enlarged image is high and the size of 2) After cold rolling, the distribution of α phase becomes much
the dimples is small, which shows a ductile fracture. The more dispersive. The tensile fractural morphology changes
features of fracture after tensile test are also in agreement with from brittle intergranular fracture to dimple fracture.
the elongation variation of different rolling reductions. It can be 3) The sheet with 70% thickness reduction possesses the
concluded that the large deformation is accompanied by the pile- ultimate tensile strength of 212 MPa, elongation of 9.4% and
up of dislocation and the dynamic recrystallization. microhardness of 60.12 HV. When the total rolling reduction
is 90%, the tensile strength decreases to 210 MPa, but the
elongation increases sharply to 19.8%.
4. Conclusions 4) Strengthening mechanisms of the cold rolled Mg–14Li–1Zn
alloy are attributed to strain hardening and grain refinement.
Strain hardening plays an important role in the enhance-
1) As-cast and as-homogenized Mg–14Li–1Zn alloy is mainly ment of strength. Grain refinement and the appropriate
composed of β phase with trace amount of tiny α phase particles. distribution of the α(Mg) can obviously improve the plasticity.

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