j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6

Available online at www.sciencedirect.com

journal homepage: www.elsevier.com/locate/jmrt

Review Article

A review of Mg alloys containing long-period

stacking ordered (LPSO) structures with insight into
the application of friction stir processing

Mohammad Saleh Geshani 1, Parastoo Mahmoud Kalayeh 1,

Amir Hossein Asadi 1, Hamed Mirzadeh*, Mehdi Malekan,
Massoud Emamy
School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran, Iran

article info abstract

Article history: Owing to their excellent mechanical/functional properties, the lightweight magnesium
Received 9 March 2023 alloys containing long-period stacking ordered (LPSO) structures have recently received a
Accepted 12 April 2023 great deal of attention. In the present overview article, the atomic structures, formation
Available online 15 April 2023 mechanisms, transformations of 18R and 14H phases, and morphology of LPSO phases in
various Mg-based systems containing special rare earth elements (such as Y and Gd) and
Keywords: transition metal elements (such as Zn, Ni, and Cu) are reviewed. Then, the effects of
Magnesium alloys thermomechanical processing and severe plastic deformation (SPD) techniques on the
Long-period stacking ordered grain refinement of the a-Mg matrix by dynamic recrystallization (DRX), kinking as the
structures main deformation mechanism of the LPSO phase, as well as the fragmentation and
Friction stir processing dispersion of LPSO phase are summarized. Afterward, the reported works on the applica-
Thermomechanical processing tion of friction stir processing (FSP) and friction stir welding (FSW) for the processing of
Mechanical properties LPSO-containing Mg alloys regarding the microstructural evolution, mechanical properties,
and strengthening mechanisms are critically discussed. Finally, distinct suggestions for
future works are proposed, including the investigation of the kinetics of the LPSO phase
formation, fabricating by the emerging processing technologies such as additive
manufacturing (AM), evaluating the FSP processing parameters (especially multi-pass FSP
and applying the Zener-Hollomon parameter), characterizing the DRX mechanisms (such
as discontinuous, continuous, and twinning-induced DRX, as well as the particle stimu-
lated nucleation for texture weakening), and studying the superplasticity and superplastic
forming of LPSO containing Mg alloys during hot deformation.
© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY license (http://creativecommons.org/licenses/by/4.0/).

* Corresponding author. School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran, Iran.
E-mail address: hmirzadeh@ut.ac.ir (H. Mirzadeh).
1
These authors contributed equally to this work.
https://doi.org/10.1016/j.jmrt.2023.04.105
2238-7854/© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://
creativecommons.org/licenses/by/4.0/).
4946 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
1. Introduction
Conventional magnesium alloys have several limitations such
as poor strength-ductility balance, low corrosion resistance,
low thermal stability, and inappropriate elevated-temperature
mechanical properties [1e3]. To overcome these issues,
methods such as modifying the chemical composition [4e6],
homogenization [7,8], precipitation hardening [9,10], compos-
ite strengthening [11,12], texture modification [13e15], and
grain refinement [16e18] have found to be effective.
Regarding the chemical composition, the addition of
special rare earth elements (RE, such as Y and Gd) to Mg
alloys that contain transition metal elements (TM, such as
Zn, Ni, and Cu) is a promising approach to overcome these
limitations. These alloying elements lead to the formation
of chemically/stacking ordered structures with favorable
attributes such as developing a coherent interface with the
matrix, deformability and kinking, high thermal stability, as
well as high strength and stiffness. These are known as the
long-period stacking ordered (LPSO) structures [19e23],
which have gained significant interest from researchers
around the world, and considerable progress is expected in
the future.
Grain refinement is one of the most effective and widely-
used methods to improve the ductility of as-cast Mg alloys,
where the significant improvement of strength is the other
main advantage. To this end, various methods during solidi-
fication [24e26], as well as thermomechanical processing
routes [27,28] and severe plastic deformation methods [29e31]
in the solid state can be used. Besides the enhancement of
strength by grain refinement (as can be represented by the
Hall-Petch law [32,33]), the improvement of ductility can be
achieved by the activation of secondary slip systems [34] as
Fig. 1 e Structure models of the MgeZneY LPSO polytype structures [41] and some representative high-angle annular dark-
field scanning transmission electron microscopy (HAADF-STEM) images [42].
well as the fragmentation and dispersion of second-phase
particles (especially the eutectic constituents) [35].
Grain refinement in Mg alloys and the resulting improve-
ments in the microstructure and properties can be readily
obtained by the friction stir processing (FSP) technique. Severe
plastic deformation at elevated temperatures generated by
FSP can refine grains, dissolve the secondary phases, refine
particles, and alleviate severe solute segregation in cast
magnesium alloys. Moreover, the temperature, deformation,
and cooling rate during FSP can be varied by controlling the
process parameter, e.g., the rotation rate and traverse speed
[36e39]. Eliminating the solute segregation in castings and
enhancing the precipitation of the LPSO phase might lead to
the distribution of the LPSO phase within the grains [40].
Therefore, FSP is an ideal method for the processing of Mg
alloys containing LPSO phases, which needs to be summa-
rized to unravel its merits.
Accordingly, in the following sections, firstly, the LPSO
structures, their formation, the corresponding Mg alloy sys-
tems, and the response of these Mg alloys to thermo-
mechanical processing are reviewed. Afterward, the reported
works on the application of FSP for the processing of Mg alloys
containing LPSO phases are critically discussed. And finally,
distinct suggestions for future works are proposed.
2. Magnesium alloys containing LPSO
phases
2.1. Types of LPSO structures
A wide range of LPSO structures has been discovered,
including 10H, 14H, 12R, 18R, and 24R [41,42]. The letters H and
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6 4947

R denote the hexahedral and rhomboid symmetries, respec-

tively. The integers indicate the number of atomic layers in a
unit cell of LPSO. Structure models of these LPSO polytype
structures are schematically shown in Fig. 1 [41]. Various
numbers of close-packed planes and different stacking se-
quences of the building block can be seen in this figure. Notice
the arrangement in opposite directions of the -ABCA-building
blocks in the 10H and 14H structures but the same shear di-
rection in the 18R and 24R structures. The most common LPSO
structures are 14H and 18R.

2.2. Formation of LPSO phases in Mg alloys

The 18R and 14H LPSO phases are usually formed during so-
lidification and elevated-temperature solid-state reactions,
respectively. The blocky 18R phase forms on the grain
boundaries of as-cast alloys in the form of a quasi-continuous
network. During solidification, due to the formation of a-Mg
grains, the solute RE and TM atoms are rejected into the liquid,
and the RE/TM concentration ratio in the liquid reaches that
needed for the 18R-phase [43]. Based on the general viewpoint
on the formation of the LPSO phase in the solid state (such as
lamellar 14H), the generation of ordered stacking faults (SFs),
diffusion of RE and TM atoms into SFs, and growth by the
ledge mechanism are the main steps in the formation of LPSO
phases [44]. In a more recent viewpoint, the nucleation of an
LPSO unit building block starts with the co-segregation of TM/
RE atoms into two adjacent closely packed layers (formation
of GP zone that is a thin basal plane defect with HCP structure
enriched by TM/RE atoms [44]) with the subsequent formation
of stacking fault to release the resultant increased energy in
the HCP structure, as schematically shown in Fig. 2. After-
ward, solute atoms tend to segregate into the newly formed
stacking faults because they are energetically favorable sites
[42]. In this way, the LPSO phase is formed in the matrix via
the reaction of supersaturated a-Mg / a-Mg þ 14H.
The 18R phase can gradually transform into the 14H phase
during the heat treatment cycle, as shown in Fig. 3 [45].
Firstly, the TM/RE atoms diffuse from the 18R phase into the
Mg matrix and form a supersaturated solid solution during
elevated-temperature exposure. This enrichment lowers the
Fig. 3 e Schematic model showing the formation of 14H
LPSO from 18R LPSO [45].
energy threshold of SFs formation on the basal planes fol-
lowed by transforming dislocation into SFs (similar to Fig. 2).
Finally, during the cooling stage, the TM/RE atoms precipitate
in SFs due to the decrease in their solid solubility in the
matrix, and hence, the 14H LPSO phase can be formed in the
grain interior [45]. In fact, two Shockley partials glide on two
adjacent planes of the 18R structure, leading to an upward
shift of -ABCA- 18R building block by one atomic layer and its
stacking sequence becomes -ACBA-. Then, via a concomitant
shuffle of Y and Zn atoms, a single unit cell of 14H could be
formed [19].
2.3. Mg-based systems containing LPSO phases
In 2001, Kawamura et al. [46] developed an Mg97Y2Zn1 alloy
with yield stress and total elongation of 610 MPa and 5%,
respectively. Since then, LPSO-containing alloys have been
widely studied. As a result, several Mg-based systems have

Fig. 2 e Schematic model showing the formation and growth of a unit LPSO phase [42].
4948 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6

been developed; among them, the MgeYeZn, MgeGdeZn,

MgeGdeYeZn, and MgeYeNi are the most investigated ones.
For the renowned MgeYeZn system, the Y/Zn atomic ratio is
an important parameter in the formation of phases [20,21],
such as 18R LPSO (Mg10YZn and Mg29Y4Zn3), 14H LPSO
(Mg12YZn and Mg35Y4Zn3), I-phase (Mg3YZn6), W-phase
(Mg3Y2Zn3), and Mg24Y5. Decreasing the Y/Zn atomic ratio
from 3.71 to 0.67 results in the phase composition of the al-
loys following the sequence of a-Mg þ LPSO þ Mg24Y5 (Y/
Zn > 2) / a-Mg þ LPSO (Y/Zn z 2) / a-Mg þ LPSO þ W-
phase (1< Y/Zn < 2) / a-Mg þ W-phase (Y/Zn < 1) [47e49]. At
lower Y/Zn atomic ratios, I-phase and other Zn-rich phases
such MgZn appear in the microstructure [20,21]. SEM images
of the common phases observed in the MgeYeZn ternary
system are shown in Fig. 4 [50,51], where the indicated Y/Zn
atomic ratios support the above statements. At a fixed Y/Zn
atomic ratio, increasing the contents of Y and Zn compared
to Mg leads to an increase in the volume fraction of LSPO in
the alloy [52]. Added to this, the stoichiometry of the LPSO
phases (MgxYyZnz) has been a subject of controversy. For Fig. 5 e Composition range of MgeYeZn LPSO phases [20].
instance, y/z ratios of 1 and 4/3 were identified above. A wide

composition range has been indicated for LPSO phases, as

shown in Fig. 5 for the MgeYeZn system [20].
The Mg-Gd-Zn system offers a unique opportunity for
exploiting precipitation hardening besides the favorable ef-
fects of LPSO phases. For instance, Fig. 6 shows the time-
etemperature-transformation (TTT) diagram for the
Mg97Zn1Gd2 alloy, showing the different precipitation se-
quences at low, medium, and high temperatures [53]. It can
be seen that a remarkable strengthening effect can be ob-
tained by aging at an appropriate temperature. In this sys-
tem, the (Mg,Zn)3Gd eutectics, I-phase (Mg3Zn6Gd), W-phase
(Mg3Zn3Gd2), 14H LPSO (Mg12ZnGd), as well as b΄0 , b΄ (Mg7Gd),
b1, b (Mg5Gd) for precipitation strengthening have been re-
ported. During elevated-temperature exposure, the lamellar
and blocky 14H LPSO form by precipitation from the solute-
enriched g0 -SFs and transformation from (Mg,Zn)3Gd phase,
respectively [53]. The 14H phase (commonly) and 18R phase
(rarely) might form in the as-cast alloy [54]. The microstruc-
tures of as-cast and solution-treated Mg96.5Gd2.5Zn1 alloy are
shown in Fig. 7, indicating the formation of the 14H phase in
the as-cast condition as well as lamellar and blocky 14H
phase in the solution-treated one [54].
For the MgeGdeYeZn system, a combination of phases
observed in MgeYeZn and MgeGdeZn systems are frequently
formed, whereby adjusting the Gd/Y ratio in the chemical
composition of the alloy, it is possible to control the micro-
structure and mechanical properties. In alloys with low Gd/Y
ratio, most of the LPSO phase forms during solidification (18R
LPSO phase); while in alloys with high Gd/Y ratio, the (Mg,Zn)3RE
eutectic phase forms (instead of the LPSO phase) that transform
to 14H LPSO phase during heat treatment [55e57]. Usually, the
Gd/Y atomic ratios higher than 1 are considered, which is ad-
vantageous concerning the enhancement of mechanical prop-
erties via precipitation strengthening. In these systems, the
presence of Y improves the age-hardening capacity of the alloy
Fig. 4 e SEM images of the common phases in MgeYeZn by promoting the precipitation of the dense b0 phase in the
ternary system [50,51]. matrix [58,59], as shown in Fig. 8.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
Fig. 6 e Timeetemperature-transformation diagram and precipitation hardening behavior of Mg97Zn1Gd2 alloy [53].
While most studied LPSO-containing alloys are based on
Zn as the TM element, there is another promising system
based on Ni as the TM element, i.e. MgeYeNi alloys with good
mechanical properties. Substitution of Zn with Ni is effective
in promoting the formation of LPSO phases, which arises from
the fact that Ni has almost zero solubility in Mg (contrary to
Zn) [60e64]. Common phases in this system are Mg2Ni,
Mg24Y5, and 18R/14H LPSO [60,62,65e68]; although the
strengthening b΄ (Mg7Y) phase might also form during aging at
intermediate temperatures such as 473 K [69e71]. In the as-
cast MgeYeNi alloys, the Y/Ni atomic ratio determines the
constituting phases. For Y/Ni > 2, in addition to the LPSO
phase, the Mg24Y5 phase is formed inside grains; while the
Mg2Ni phase is formed at grain boundaries for lower Y/Ni
values [60,72]. The effect of the Y/Ni ratio (in the composition
of the alloy) on phase formation can be seen in Fig. 9 [60,61].
Recently, solute-enriched g0 -SFs have been detected in the
microstructure of solidified MgeNieY alloys at a high cooling
rate for supersaturation of Y and Ni [61], as shown in Fig. 9,
which implies that heat treatment might lead to the formation
Fig. 7 e SEM images of as-cast and solution-treated
Mg96.5Gd2.5Zn1 alloy [54].
4949
of 14H LPSO [63,73], similar to the mechanism indicated in
Fig. 3.
The LPSO phases in the MgeYeNi system have the same
structure as the phases in the MgeYeZn system [74], and
hence, the diffraction peaks of LPSO phases can be indexed
based on reported data for the MgeYeZn alloys [72,75], as
shown in Fig. 10 [65]. Another important aspect is the high
thermal stability of LPSO phases in the MgeREeNi systems.
For instance, in the MgeGdeNi alloys, a structural trans-
formation from 18R to 14H was observed, but it was hardly
dissolved into the a-Mg matrix [76].
Other transition metals (TM) such as Co and Cu can form
LPSO phases. For instance, LPSO phases have been observed in
MgeYeCo [77,78] and MgeYeCu [79] alloys. Besides transition
metals, Al as a post-transition metal can form LPSO phases in
MgeYeAl [80] and Mg-Gd-Al [81] systems. Other RE elements
such as Dy and Er have also been indicated in MgeDyeZn [82]
and MgeEreZn [83] systems, respectively.
2.4. Thermomechanical processing of Mg alloys
containing LPSO phases
Thermomechanical processing is an effective way to refine
the microstructure, modifying the morphology, distribution,
and amount of phases, closure of casting defects, and altering
the texture for the improvement of mechanical properties
[19,84e86]. Dynamic recrystallization (DRX) is a potent resto-
ration process during hot working, for which the evolution of
the microstructure depends on the initial grain size and
structure, as well as the deformation conditions such as
temperature, strain rate, and strain [87,88]. The DRX grain size
(dDRX) is mainly controlled by the Zener-Hollomon parameter
Z ¼ ε_ expðQdef =RTÞ via dDRX ¼ AZp [89], where Qdef is the
deformation activation energy, and A and p are constants.
While Qdef is normally close to the lattice diffusion activation
energy in Mg (135 kJ/mol) for many Mg alloys [90], high values
of Qdef (in the range of 250e400 kJ/mol) have been reported for
Mg alloys containing LPSO phases [91e95]. This has been
related to the presence of intragranular thin-platelet LPSO
phases with high thermal stability, which are effective bar-
riers to the deformation process, providing back stress, and
4950 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
Fig. 8 e Age hardening curves of MgeGdeYeZneMn alloys
[58].
inhibiting lattice rotation of the matrix [92,95]. Therefore, the
presence of LPSO phases is important during hot working.
During deformation, the original fine lamellae of the 14H LPSO
phase change to the bent lamellae, followed by the formation
of zigzag kink bands and cracked lamellae, and finally rect-
angular microcells are formed in the matrix, as schematically
shown in Fig. 11a [96]. The original lathes of the 18R LPSO
phase are bent and kinked, followed by cracking and delami-
nation, and final fragmentation to small 18R particles, as
schematically illustrated in Fig. 11b [97]. The fragmented
Fig. 9 e SEM images of as-cast MeNieY alloys, HADDF-STEM image, and elemental mappings of g′phase [60,61].
particles usually align along the deformation direction [98]. It
can be seen in Fig. 11 that kinking is the main deformation
mechanism of the LPSO phase. Similar to the a-Mg matrix, the
ð0001ÞC1120D basal slip is the main deformation mechanism for
the LPSO phase. However, in the case of difficulty for basal
slip, kink deformation is initiated by progressive rotation of
the lattice via dislocation dipole-pair generations within grain
interiors followed by generation of a pair of kink interfaces
composed of opposite edge dislocations with a stepwise
shape, as shown in Fig. 12 by a schematic and some repre-
sentative SEM and TEM images [19,73,99e102]. Besides step-
wise kinking, there is rotational kinking, which results in the
relevant interfaces with the same rotational direction, as
shown in Fig. 12 [99].
The kinking process promotes the accumulation of dislo-
cations (kink boundaries play the same role as grain bound-
aries), and hence, it contributes to the improvement of
strength. Moreover, with a Young modulus twice that of the
matrix, LPSO phases with high hardness can bear the load
transferred from the matrix through the coherent interface
[19,64,105]. On the other hand, kink bands in the LPSO phase
are effective in the enhancement of ductility by generating
homogenous strain in crystals and inhibiting the initiation and
propagation of microcracks [84,96,102,106,107]. It is note-
worthy that the addition of rare earth metals (such as Y and Gd)
tends to hinder twin formation, so the deformability of the
LPSO phase is attained by the formation of kink bands [21].
The presence of blocky and/or lamellar LPSO phases can
significantly affect the DRX process [19,43,65,85]. The heavily
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
Fig. 10 e XRD patterns of different LPSOecontaining Mg
alloys [65].
deformed zones at a-MgeLPSO interfaces tend to generate
DRX grains during thermomechanical processing via the
particle stimulated nucleation (PSN) mechanism. While this is
the case for the intergranular blocky 18R LPSO phases, the
intragranular thin 14H LPSO plates tend to restrict DRX by
restraining lattice rotation of a-Mg grains and hindering
migration of boundaries of DRX. However, via 14H kinking
during deformation, the kink-aided DRX (KDRX) can be grad-
ually promoted due to the relaxation of the local strain near
kink boundaries and accommodation of relatively large plastic
deformation. Moreover, fragmentation of the 14H lamellae to
fine particles may further stimulate DRX (as shown in the SEM
image and electron backscatter diffraction (EBSD) map of
Fig. 13 [106]). Accordingly, a mixed microstructure with LPSO
particles and DRX grains might be generated at the end [19], as
schematically shown in Fig. 13 [108]. It is noteworthy that the
grain orientation spread (GOS) can be used to separate the
recrystallized grains from the deformed ones [109,110].
It should be noted that complete DRX is usually not
attained for LPSO-containing alloys under conventional
Fig. 11 e Schematics for morphological evolution of LPSO phases during thermomechanical processing: (a) 14H LPSO and (b)
18R LPSO phases [96,97].
4951
Fig. 12 e Schematic illustrations of kink deformation and
representative images of LPSO deformation and kinking
[99,103,104].
thermomechanical processing routes. Moreover, the LPSO
phase shows good ductility and tends to be kinked but not
refined. The strengthening effect of the LPSO phase can be
enhanced when it is refined to a micron or submicron level
[19]. Accordingly, SPD at elevated temperatures might be
considered a good solution for this purpose. In this regard, Xu
et al. [111] reported that the grain refinement of Mg-
9Gde3Ye2Zne0.5Zr alloy by the reciprocating upsetting-
extrusion (RUE) severe plastic deformation method is effec-
tive in the improvement of strength-ductility balance, as
shown in Fig. 14. While the enhancement of both strength and
ductility is evident, it can be seen that the LPSO phase has
been partially refined [111]. For better refinement of second-
phase particles, processes such as FSP/FSW (friction stir
welding) showed promising results [112e115]. They are able to
impart large deformations at elevated temperatures in one
pass for the promotion of DRX and fragmentation and
dispersion of particles [116e120]. Therefore, the FSP has been
considered in the following sections.
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Fig. 13 e Schematic illustrations of DRX during thermomechanical processing of Mg alloy containing LPSO phases [108], as
well as SEM image and EBSD map representing the occurrence of KDRX [106].

Fig. 14 e Inverse pole figure EBSD maps and SEM image of RUE-processed Mge9Gde3Ye2Zne0.5Zr alloy and the summary
of room-temperature tensile properties [111].
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6 4953

point, ε_ is the estimated strain rate during FSP, 0.04  a  0.06,

3. Friction stir processing of Mg alloys and 0.65  K  0.75. Also, Rn and Dn are the effective (or
containing LPSO phases average) radius and depth of the dynamically recrystallized
zone [138e141].
Friction stir processing (FSP) is applied by pushing a rotating Accordingly, similar to hot deformation studies, the Zener-
tool (consisting of a pin and a shoulder) into the surface fol- Hollomon parameter can be estimated by Z ¼ ε_ expðQ =RTÞ,
lowed by its translational movement, which leads to the local where Q is similar to the lattice self-diffusion (135 kJ/mol for
softening of the material (due to the frictional/adiabatic
Mg alloys) [87,142e144]. Finally, the equation d ¼ AZB is used
heating), mixing, and deformation [121]. Accordingly, the
to relate d with Z. Clearly FSP with external cooling accentu-
grain refinement induced by DRX [36,122,123] as well as the
ates grain refinement due to the decreased T, as well as the
alteration of the amount, morphology, and distribution of
inhibition of extensive grain growth and dissolution of pre-
particles [112,124e127] might lead to a pronounced improve-
cipitates in and around the stirred zone [121,145e149].
ment of properties such as mechanical properties
Regarding the Mg alloys containing LPSO phases, there are
[112,128e131] and the possibility to achieve superplasticity
several reported works, which are summarized in the
[116,132]. Various DRX mechanisms such as discontinuous
following.
(DDRX), continuous (CDRX), geometric (GDRX), and twinning-
The most studied alloys are based on the
induced DRX (TDRX) have been reported as the mechanisms
MgeGdeYeZneZr system. Yang et al. [40] investigated the
for grain refinement [17,116,122]. DDRX involves a two-step
effects of heat and deformation conditions on the distribution
process, i.e. the nucleation of new grains surrounded by
of the LPSO phase during FSP of an MgeGdeYeZneZr alloy.
high-angle grain boundaries followed by their growth by
Grain refinement, elimination of Mg3RE eutectics, and for-
means of long-range migration. In contrast, CDRX involves
mation of fine lamellar LPSO phase were observed during FSP.
the gradual transformation of the dislocation sub-boundaries
In fact, the LPSO phase forms (1) at the grain boundaries via
produced at low strains into ultrafine grains with high angle
transformation from b phase at above 425  C (~700 K) and (2)
boundaries at large strains [16,17]. GDRX involves the serra-
precipitates at the grain boundaries and within the grains
tion of grain boundaries during dynamic recovery, flattening
from the supersaturated matrix at above 350  C (623 K) with
of grains, interpenetration of the scalloped boundaries, and
the LPSO lamellae developing on the bases of stacking faults,
formation of a microstructure of small equiaxed grains of a
size comparable with the subgrain size [16]. Finally, in TDRX,
twinning plays an important role in the DRX process.
From the stir zone (SZ) to the base metal (BM), a thermo-
mechanically affected zone (TMAZ) and a heat-affected zone
(HAZ) also develop. TMAZ is quite important in FSP [112] and
knowledge regarding the microstructural evolution in HAZ is
vital for controlling the properties of the welding parts
[133,134]. The primary processing parameters include tool
geometry, tool rotation rate (u), and traverse speed (v) [116]. A
higher u or lower v normally leads to a higher temperature (T)
during FSP [135]. Adequate heating is always required to pro-
duce a defect-free nugget with the refined microstructure
[136], but a common observation is the refinement of the
dynamically recrystallized grain size (d) by decreasing u at
constant v or increasing v at constant u [137]. In fact, T= Tm z
Kðu2 =v  104 Þa and ε_ zpu  Rn =Dn , where Tm is the melting

Fig. 15 e Temperature histories of the FSP Mg-Gd-Y-Zn-Zr Fig. 16 e Variation of grain size with the FSP parameters for
casting [40]. the MgeGdeYeZneZr casting alloy [40].
4954 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
Fig. 17 e Tensile stress-strain curves, microstructures,
fracture surface appearances of as-cast and FSP
MgeGdeYeZneZr alloy [150].
and growing and coarsening with increasing annealing time
and temperature [40]. The presence of phases at these tem-
peratures is consistent with the predictions of Fig. 6.
Yang et al. [40] also argued that the distribution of the LSPO
phase is dependent on the FSP processing parameters and the
Fig. 18 e Multi-pass FSP of MgeGdeYeZneZr alloy with overlapping and the resulting mechanical properties and
strengthening mechanisms [151].
processed regions due to the change in temperature, plastic
strain, and cooling rate. The temperature history during FSP
for the bottom region of the stir zone is shown in Fig. 15. It can
be seen that FSP is able to increase the temperature to higher
than 600 K, which is the required temperature for the disso-
lution of Mg3RE eutectics and formation of the LPSO phase, as
shown in Fig. 6. Moreover, by increasing the rotation rate
(A/C/D), the peak temperature and exposure time at tem-
peratures higher than 600 K increase and a higher plastic
strain is imposed on the material. However, by increasing the
traverse speed (C/B), the peak temperature, the exposure
time, and the plastic strain decrease; while the cooling rate
increases. Furthermore, the temperature decreases by moving
from the top region to the bottom; while the plastic strain
initially decreases by moving from the top to the middle re-
gion and then increases to its maximum value by moving to
the bottom of the stir zone. Accordingly, the temperature and
the plastic strain can be adjusted by the FSP parameters,
which affect the distribution of phases.
Regarding grain refinement, Yang et al. [40] also showed
that a lower u or higher v leads to more intense grain refine-
ment, as shown in Fig. 16. Moreover, by moving from the top
of the stir zone to its bottom, the grain size is refined. All of
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6 4955

these observations can be explained by the change in the heat
input. In a related work, Yang et al. [150] also showed that FSP
of this alloy leads to a significant improvement of tensile
properties as well as the change in the fracture surface
appearance from the cleavage (brittle) to dimple (ductile)
appearance, as summarized in Fig. 17. These improvements
were mainly related to the intense grain refinement (from 97
to 2.4 mm) and the replacement of the large grain boundary
particle networks in the as-cast condition by fine LPSO
lamellae (with a width of 5e200 nm) within grains.
Regarding the strengthening mechanisms of the
MgeGdeYeZneZr alloy after multi-pass FSP with overlapping
strategy (Fig. 18a), Guan et al. [151] considered two distinct
tensile samples: a tensile sample from the interfacial zone
(the area overlapping the TMAZ zone during the previous pass
and subsequent pass) and a tensile sample from the processed
zone. In the processed zone, a grain size of 3 ± 1.2 mm, a high
angle grain boundary fraction of ~93%, a broken blocky 18R
LPSO phase, and a low fraction of needle-like 14H LPSO phase
were observed. However, in the interfacial zone, a grain size of

Fig. 19 e (a) EBSD map of the FSP MgeGdeYeZneZn alloy, (b) the corresponding boundary misorientation distribution
histogram, (c) tensile specimens pulled to failure, (d) variation of elongation with initial strain rate, and (e) variation of flow
stress with initial strain rate [117].
4956 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6

4 ± 2.5 mm, a high angle grain boundary fraction of ~93%,
smaller and more dispersed broken blocky 18R LPSO phase,
and a much higher fraction of needle-like 14H LPSO phase
were observed. Regarding the higher amount of the 14H LPSO
phase in the interfacial zone, the shear deformation caused by
the edge of the stirring pin along the transverse direction (TD)
promotes the generation and movement of numerous partial
dislocations (stacking fault) in the interfacial zone and
provides favorable conditions for the structural trans-
formation of the LPSO phase. In addition, the short-range
diffusion promotes the shuffling of Zn and RE atoms during
multi-pass FSP. Accordingly, in a shorter time and at lower
temperatures compared to those required for the heat treat-
ment, the phase transformation from 18R to 14H LPSO can be
achieved, which prevents the coarsening of the LPSO phase
and grain growth. As shown in Fig. 18b, the mechanical

Fig. 20 e Microstructures of SZ, TMAZ, and BM for the FSP MgeGdeYeZneZn alloy [159].

Fig. 21 e Summary of mechanical properties of FSP MgeGdeYeZneZn alloy before and after peak aging at 225  C [159].
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
Fig. 22 e Equilibrium phase-temperature diagram based on
thermodynamics calculation for Mge12.99Gde4Ye2Zn
alloy by JMatPro software.
properties of both samples are similar. However, as summa-
rized in Fig. 18c, the contributions of strengthening mecha-
nisms are different due to the change in the microstructure as
discussed above. For instance, the contribution of the 14H
LPSO phase is more remarkable in the interfacial zone [151].
Mg alloys containing LPSO phases might exhibit excep-
tional superplasticity [117,152e154], especially after FSP. For
instance, Yang et al. [117] showed that the FSP of
MgeGdeYeZneZr alloy using the rotation rate of 800 rpm and
traverse speed of 100 mm/min led to the grain size of 3 mm
with high angle grain boundary fraction of 97% (as shown in
Fig. 23 e Electron channeling contrast (ECC) images from BM and SZ of FSP Mge12.8Ye4.7Zn and the width of LPSO particles
in the SZ [118].
4957
Fig. 19a and b), and distributed LPSO lamellae throughout the
grains (similar to Fig. 17). The fine-grained equiaxed micro-
structures with high-angle grain boundaries to permit GBS
[155] and dispersed second-phase particles to inhibit grain
growth [156,157] are known to be essential requirements to
achieve superplasticity in Mg alloys, as recently reviewed by
Savaedi et al. [154]. Accordingly, one of the highest recorded
superplastic elongations in Mg alloys was achieved for the FSP
MgeGdeYeZneZr alloy, i.e., total elongation of 3570% at the
temperature of 425  C and strain rate of 0.03 s1, as shown in
Fig. 19c [117]. Moreover, as shown in Fig. 19d, this alloy
showed high strain rate superplasticity (at strain rates higher
than 0.01 s1). Furthermore, as shown in Fig. 19e, the strain
rate sensitivity index was also determined as ~0.6, indicating
the occurrence of grain boundary sliding (GBS) during high-
temperature deformation [154,155]. The LPSO lamellae
within grains led to high thermal stability, and the high frac-
tion of high-angle boundaries facilitated GBS and accelerated
superplastic deformation kinetics [117].
For an MgeGdeYeZneZr alloy, similar to other works
[40,158], besides the effective breaking up of the LPSO phases
(see SZ and TMAZ regions shown in Fig. 20), dissolution of
eutectic Mg3(Gd,Y) phase in the SZ region, and precipitation of
lamellar 14H LPSO phase in the interior of DRX grains, Li et at.
[159] also observed the formation of the b-Mg5(Gd,Y) at triple
junctions of the DRX grains during FSP, as shown in Fig. 21.
The presence and formation of this phase and other phases
can also be confirmed based on the JMatPro plot shown in
Fig. 22. The tiny particles obtained by the drastic stirring effect
increased the number of DRX nucleation sites through the
particle stimulated nucleation (PSN) mechanism, which also
has been confirmed by Shahsa et al. [160]. Moreover, the
4958 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
dissolution of the eutectic Mg3(Gd,Y) phase provided the RE
elements for the precipitation of the 14H LPSO phase. Conse-
quently, the 18R LPSO phase is transformed into numerous
needle-like 14H LPSO phases. Li et at. [159] also showed that
the FSP MgeGdeYeZneZr alloy has a remarkable age-
hardening capability during subsequent aging at 225  C
(498 K) due to the precipitation of b0 phase, which is summa-
rized in Fig. 21.
Besides the most studied alloying system
(MgeGdeYeZneZr alloys), Li et al. [119] studied the micro-
structure and mechanical behavior of FSPed Mg-14Gd-2.3Zn-
0.6Zr (wt%) alloy. They reported that FSP led to the breaking
up of the coarse LPSO phase at grain boundaries into fine
particles (~1 mm) and significant refinement of the grain size
from 23 to 1.6 mm through DRX. These microstructural im-
provements resulted in the increment of the yield strength by
~30%; while the elongation decreased by ~39% because of the
heterogeneous microstructure. In another study, for the
Mge12.8Ye4.7Zn (wt%) alloy with a very high content of
coarse LPSO phases, Li et al. [118] used FSP for refining the
Fig. 24 e Microstructures of as-cast Mg95.8Zn3.6Gd0.6 and Mg97Cu1Y2 (at%) alloys and after dissimilar FSW representing the
formation of onion ring structure as well as L1 and L2 layers [161].
coarse LPSO phases into densely ultrafine blocks with an
average width of ~200 nm and an average length of ~1 mm
(Fig. 23). Accordingly, ultrahigh compressive yield strength of
~800 MPa was achieved, for which the contribution of the
densely ultrafine LPSO phases was up to ~630 MPa. These
authors proposed that FSP is a viable approach for the
refinement of LPSO phases, which are hard to break during
traditional plastic processing such as extrusion, rolling, and
forging due to their plasticity via kinking deformation or the
need for the high number of passes in methods such as equal-
channel angular pressing (ECAP).
Liang et al. [161] investigated the mixing of Mg95.8Zn3.6Gd0.6
and Mg97Cu1Y2 (at%) alloys during dissimilar FSW. A lami-
nated onion-ring structure composed of alternative distribu-
tion of L1 and L2 layers was formed in the SZ, as shown in
Fig. 24. In the L1 layer corresponding to the Mg95.8Zn3.6Gd0.6
alloy, the I-phase is broken up and dispersed with most of
them being transformed into cubic W-phase particles, and the
grain size was in the range of 1e4 mm. Moreover, in the L2 layer
corresponding to the Mg97Cu1Y2 alloy, the thick 18R LPSO
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6 4959

microstructural refinement resulted in UTS of 415 MPa and an

elongation to failure of ~28%, both exceeding those obtained
for the base materials.
Fine grain size, low dislocation density, and weak crystal-
lographic texture are crucial for the improvement of the
comprehensive performance of Mg alloys as the anode for Mg-
air batteries. However, this unique microstructure can hardly
be achieved with conventional plastic deformation techniques
such as rolling or extrusion combined with annealing.
Accordingly, in a recent study, Liu et al. [162] tailored the
microstructure of MgeAleSneRE alloy by applying FSP, for
which all of the above requirements were achieved and higher
discharge voltages and capacities were obtained compared to
those obtained for the untreated anode. Moreover, the frac-
tured LPSO and other phases effectively inhibited the micro-
galvanic effect and spalling of oxidation products. Further-
more, compared with the homogenized alloy with larger grains
and second phases, FSP showed a lower rate of hydrogen
evolution when discharged at the same current density.
Fig. 25 e (a) Effect of aging time on the conductivity of
Mg95.5Zn1.5Y3 alloy and (b) JMAK analysis [163].
4. Summary and future prospects

plates were fractured and transformed into fine 14H LPSO In the previous sections, the Mg alloys containing LPSO phases
lamellae and the grain size was in the range of 0.6e1.8 mm. The were reviewed and the reported results on the application of
formation of the laminated structure and significant FSP for the processing of these alloys were analyzed. It can be

Fig. 26 e Schematic of 14H-LPSO phase formation process during heat treatment of additively manufactured Mge5Zne10Gd
alloy as well as some representative bright-field TEM images [165].
4960 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 9 4 5 e4 9 6 6
seen that significant progress has been made so far. However,
there remains a lot of research prospects and a lack of
knowledge, which needs much more focus on the subject.
Accordingly, the research prospects are summarized below.
While there are many reported works on the formation of
the LPSO phase in several systems, the kinetics of the LPSO
phase formation has received less attention. For instance, the
aging kinetics of 14H-LPSO precipitates in Mg95.5Zn1.5Y3 alloy
has been studied by the electrical conductivity (Fig. 25a), and
the equation of f ¼ 1-exp (-0.2705t0.6368) was obtained by the
JohnsoneMehleAvramieKolmogorov (JMAK) analysis
(Fig. 25b) [163]. As reviewed in the present article, the volume
fraction of the phases is quite important for adjusting the
properties [164], and it can be controlled during processing.
Accordingly, more studies on the kinetics of the LPSO phase
formation are needed. Moreover, the emerging processing
technologies such as additive manufacturing (AM) can also be
used to manufacture LPSO containing Mg alloys [165,166],
which need more attention. An example is shown in Fig. 26,
which shows that the as-built Mge5Zne10Gd part by laser
additive manufacturing is predominated by uniform and fine
a-Mg grains along with reticular (Mg,Zn)3Gd at grain bound-
aries. After solution heat treatment, the (Mg,Zn)3Gd phase
transformed into plate-shaped 14H-LPSO and needle-like SFs.
In the previous section, the reported works on the FSP of Mg
alloys containing LPSO phases were summarized, which are
MgeGdeYeZneZr, MgeGdeZneZr, MgeYeZn, MgeGdeZn,
MgeYeCu, and MgeAleSneRE. Another major system is the
MgeNi-RE alloys, which showed even better performance
compared to the MgeZneRE alloys. However, to the best of the
authors’ knowledge, there is no reported work on the FSP of this
system. Moreover, only one research has been conducted on the
renowned MgeZneRE alloys so far [118]. Other notable systems
that need to be investigated are MgeREeCo, MgeDyeZn,
MgeEreZn, and MgeREeAl. Moreover, since the phase compo-
sition is dependent on the atomic RE/TM ratio, altering this ratio
and investigating its effects on the microstructural evolution
(grain size and evolution of phases) during FSP is quite inter-
esting. Furthermore, due to the importance of the presence and
type of phases during FSP, more insight into the formation and
stability domain of phases by thermodynamics calculations and
thermal analysis provides indispensable information for
tailoring the microstructure and properties.
The processing parameters during FSP have pronounced
effects on the microstructural development and resultant
properties. In this regard, for the Mg alloys containing LPSO
phases, there are few studies investigating the effect of
different rotation rate/traverse speed ratios [40,118,150] and
multi-pass FSP [118,150,151,159]. However, there is no distinct
report on the influence of the number of FSP passes on the
microstructure and properties. It is well-known that multi-
pass FSP might have a pronounced effect on the grain size,
distribution of second-phase particles, and fraction of high-
angle grain boundaries [167,168], which need to be investi-
gated in LPSO containing Mg alloys. Moreover, external cool-
ing during FSP (e.g. submerged FSP) [169e173] and tool
geometry and process modification [174e177] have shown
significant effects on the SFPed microstructure, which need to
be investigated in Mg alloys containing LPSO phases due to the
complexities arises by the presence of LPSO phases. On the
other hand, the introduction of reinforcing particles through
the processing of surface hybrid composites by the hole filling
and groove filling methods [178e180] can also be practiced for
further improvement of mechanical properties and accentu-
ating the superplastic behavior [181]. Moreover, as shown in
Ref. [161], dissimilar FSW in the systems with various sec-
ondary phases might lead to interesting microstructures and
improved properties, and hence, it is expected that this aspect
receives more attention in the future.
Regarding the grain refining mechanisms during FSP,
several DRX mechanisms such as the CDRX, DDRX, GDRX, and
TDRX have been reported so far [36,122,123]. However, this
aspect has not been studied in LPSO containing Mg alloys.
Moreover, the presence of the LPSO phase might lead to the
PSN mechanism, which needs more investigations regarding
texture weakening and grain refinement capability [182e186].
Some Mg alloys containing LPSO phases exhibit remarkable
age-hardening behavior, which can be significantly changed
after SPD. Accordingly, the age-hardening behavior of Mg al-
loys containing LPSO phases before and after FSP should be
further studied and compared [159]. These kinds of post-
processing treatments can significantly improve the mechan-
ical properties for widening the application of these alloys.
Finally, as discussed above, Mg alloys containing LPSO
phases show remarkable superplasticity [187,188], and one of
the highest tensile elongation values in Mg alloys has been
reported [117]. Due to the diversity of the Mg alloys containing
LPSO phases, their good thermal stability, and the favorable
effects of FSP on the superplastic microstructure, much more
work on this subject based on tensile testing or more recent
techniques such as shear punch testing [189e191] is expected
in the future.
Ethical statement
The manuscript has been prepared by the contribution of all
authors, it is the original authors work, it has not been pub-
lished before, it has been solely submitted to this journal, and
if accepted, it will not be submitted to any other journal in any
language.
Funding body
This work received no funding.
Declaration of competing interest
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
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Mohammad Saleh Geshani. Master Student at the School of Met-
allurgy and Materials Engineering, College of Engineering, Uni-
versity of Tehran, P.O. Box: 11155-4563, Tehran, Iran. https://
scholar.google.com/citations?user¼apO1k0gAAAAJ&hl¼en
Parastoo Mahmoud Kalayeh. Master Student at the School of
Metallurgy and Materials Engineering, College of Engineering,
University of Tehran, P.O. Box: 11155-4563, Tehran, Iran. https://
scholar.google.com/citations?user¼yjBWVjYAAAAJ&hl¼en
Amir Hossein Asadi. Master Student at the School of Metallurgy
and Materials Engineering, College of Engineering, University of
Tehran, P.O. Box: 11155-4563, Tehran, Iran. https://scholar.google.
com/citations?user¼aN0qrNIAAAAJ&hl¼en
Hamed Mirzadeh. Associate Professor at the School of Metallurgy
and Materials Engineering, College of Engineering, University of
Tehran, P.O. Box: 11155-4563, Tehran, Iran.https://scholar.google.
com/citations?user¼1-0h_roAAAAJ&hl¼en
Mehdi Malekan. Associate Professor at the School of Metallurgy
and Materials Engineering, College of Engineering, University of
Tehran, P.O. Box: 11155-4563, Tehran, Iran.https://scholar.google.
com/citations?user¼ZFapdJcAAAAJ&hl¼en
Massoud Emamy. Professor at the School of Metallurgy and Ma-
terials Engineering, College of Engineering, University of Tehran,
P.O. Box: 11155-4563, Tehran, Iran.https://scholar.google.com/
citations?user¼1tfVCacAAAAJ&hl¼en