Materials Science & Engineering A 675 (2016) 338–344

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Materials Science & Engineering A

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

Achieving excellent thermal stability and very high activation energy

in an ultrafine-grained magnesium silver rare earth alloy prepared by
friction stir processing
F. Khan MD a, S.K. Panigrahi a,n
a
Department of Mechanical Engineering, Indian Institute of Technology Madras, Chennai 600036, India

art ic l e i nf o a b s t r a c t

Article history: Ultrafine-grained microstructure of a QE22 alloy prepared by Friction Stir processing (FSP) is isochronally
Received 26 June 2016 annealed to study the thermal stability and grain growth kinetics. The FSPed microstructure of QE22
Received in revised form alloy is thermally stable under ultrafine-grained regime up to 300 °C and the activation energy required
13 August 2016
for grain growth is found to be exceptionally high as compared to conventional ultrafine-grained mag-
Accepted 18 August 2016
Available online 20 August 2016
nesium alloys. The high thermal stability and activation energy of the FSPed QE22 alloy is due to Zener
pinning effect from thermally stable eutectic Mg12Nd and fine precipitates Mg12Nd2Ag and solute drag
Keywords: effect from segregation of Neodymium (Nd) solute atoms at grain boundaries.
Magnesium rare earth alloy & 2016 Elsevier B.V. All rights reserved.
Friction stir processing
Ultrafine-grained microstructure
Thermal stability
Solute drag effect
Zener pinning effect

1. Introduction processing microstructure, porosity, impurity, grain size distribu-

Magnesium alloys have received significant attention in aero-
space and automotive industries due to their high strength to
weight ratio, high damping performance and better creep re-
sistance [1,2]. However, due to their hexagonal closed packed
crystal structure, these magnesium alloys exhibit low room tem-
perature ductility, poor formability, yield strength anisotropy and
comparatively lower strength [3]. It is well proven that the
aforementioned properties of these alloys can be significantly
enhanced by two ways such as (i) refinement of grain structure to
the ultrafine regime which leads to enhanced strength and duc-
tility and reduced tension-compression yield asymmetry [3] and
(ii) addition of rare earth (RE) elements, which improve the
formability and ductility by weakening the texture [4–13].
Recently, many researchers have developed ultrafine-grained
(UFG) magnesium alloys using severe plastic deformation (SPD)
methods [14–29] and found superior properties in the UFG ma-
terial as compared to their base counterpart. But the practical
applications of the UFG materials are limited due to low thermal
stability of the microstructure at elevated temperatures that
complicates the processing of final products. Thermal stability
depends on many variables, such as compositional parameters,
n
Corresponding author.
E-mail address: skpanigrahi@iitm.ac.in (S.K. Panigrahi).
tion and texture [22–24,30–32]. Efforts have been made to develop
new UFG and nano-crystalline magnesium alloys having improved
thermal stability at higher temperatures by adding reinforcement
and other alloying elements [30–33]. However, extensive grain
growth have been observed above 200 °C temperature in various
nano-crystalline and UFG magnesium alloys [14–18,20,21,25,34].
The formability and ductility of magnesium alloys can also be
improved by weakening the recrystallization textures via addition
of RE elements to wrought magnesium alloys. Even though many
researchers reported that the weakening of texture happens be-
cause of segregation of RE atoms to grain boundaries, but the clear
mechanism is not well understood. [4–13]. Grain boundary seg-
regation is an extremely sensitive phenomenon that may sig-
nificantly affect the material properties like corrosion resistance,
mechanical behavior or the thermal stability. Also the role of RE
elements on thermal stability of UFG magnesium alloys is not well
understood. The main objectives of the present work are to first
develop UFG microstructure in a RE contained Mg-Ag alloy (QE22)
and then to study and correlate the role of solute drag and Zener
pinning effect on thermal stability and grain growth kinetics of the
developed UFG QE22 alloy.
2. Materials and methods
The QE22 alloy is procured from Magnesium Elektron North

http://dx.doi.org/10.1016/j.msea.2016.08.077
0921-5093/& 2016 Elsevier B.V. All rights reserved.
 F. Khan MD, S.K. Panigrahi / Materials Science & Engineering A 675 (2016) 338–344 339

America which is having chemical composition of Ag, 4.08 wt%;

Nd, 2.07 wt%; Zr, 0.6 wt%; Mg, balance. The as-received QE22
plates of 6 mm thickness were FSPed in two passes with a tool
rotation rate of 800 rpm and 600 rpm respectively and a traverse
speed of 100 mm/min. A custom designed FSP tool was used for
FSP passes with shoulder diameter of 12 mm and tapered threaded
pin of 3.4 mm length and 6 mm root diameter. In order to in-
vestigate the thermal stability and grain growth kinetics of the
UFG material, the FSPed plates were subjected to isochronal an-
nealing for 60 min at different temperatures in the range of 100–
450 °C, since most of the industrial and superplastic forming op-
erations are conducted within this range at sufficiently high strain
rates to avoid grain growth due to the prolonged thermal exposure
[14,34].
Microstructural examination was conducted using optical mi-
croscopy (OM), transmission electron microscopy (TEM) and
scanning electron microscopy (SEM). For OM and SEM character-
ization the as-received QE22 alloy samples were subjected to
mechanical polishing by using different emery grit sizes, fol-
lowed by diamond polishing and etched with picric acid solution.
An inverted metallographic optical microscope Quama 5000 series
and a Quanta 200 SEM were used for the microstructure ob-
servation. For TEM characterization a 500 mm thin foils of FSPed
samples are sliced from the processed zone using precision low
speed cutting machine and mechanically grounded to less than
80 mm. These thin foils are punched in to 3 mm disc and were ion
milled with an incident angle of 6° and an energy beam of 5 eV in
an argon environment till a transparent region is formed. Micro-
structural observation by TEM was undertaken by using Phillips-
CM12 electron microscopy operating at an accelerating voltage of
120 kV. To calculate the average grain size of the FSPed samples, a
mean linear intercept method was used by considering at least 50
unique grains in each annealing condition. The polished FSPed
samples were taken to micro-hardness testing to determine the
hardness value. The test was carried out on Future Tech FM-707
Vickers Micro-hardness testing machine with a load of 200 g for
10 s.

3. Results and discussion

3.1. Microstructural characterization of an FSPed UFG QE22 alloy

Fig. 1(A) shows the as-received cast QE22 magnesium alloy

which is composed of magnesium solid solution with equiaxed
grains surrounded by thermally stable eutectic network of Mg12Nd
(Fig. 1(B)) and precipitates of Mg12Nd2Ag (Fig. 1(C)) inside the
magnesium matrix. The average grain size and Mg12Nd eutectic
size is observed as 38 712 mm and 8.3 73.6 mm respectively and
bearing an average micro-hardness of 83 74 HV [35]. Fig. 2 shows
the TEM microstructure of the QE22 magnesium alloy after FSP at
the center of the stirred zone. The FSP resulted (i) complete
transformation of cast microstructure to uniformly distributed
equiaxed dynamic recrystallized UFG microstructure with average
grain size of 0.63 70.1 mm because of SPD during multi-pass FSP
and (ii) fragmentation of large eutectic Mg12Nd network which
was observed along the grain boundary in the cast microstructures
in to small particles with average particle size of 0.2 7 0.05 mm and
uniform distribution of these particles along the grain boundaries
as well as at triple point junctions of the grain boundaries and (iii)
dissolution of Mg12Nd2Ag precipitate in magnesium matrix.
Fig. 3 shows the TEM microstructures after isochronal anneal-
ing treatment for 60 min at different temperatures. During an-
nealing process Mg12Nd2Ag precipitates are formed like a con-
tinuous chain along the grain boundary as shown in Fig. 3(B-D).
The average grain size, particle size and micro-hardness are
Fig. 1. Microstructure of an as-received cast QE22 magnesium alloy. (A) Optical
micrograph showing equiaxed microstructure (B) Back scattered electron (BSE)
micrograph; arrow indicates the Mg12Nd eutectic (C) TEM micrograph showing
Mg12Nd2Ag precipitates.
plotted against the annealing temperature in Fig. 4. At low-tem-
perature region (100–300 °C) of annealing treatment, there is al-
most negligible increase in grain and eutectic particle sizes
(Mg12Nd). A slight increasing trend of both grain size and eutectics
is observed at high annealing temperature region (300–450 °C).
The grain size retained in UFG regime upto 300 °C and increases
upto
3.8 mm at 450 °C temperature shown in Fig. 5.
The micro-hardness of UFG QE22 sample is slightly decreased
when annealed in the range of 100–300 °C, although microscopy
studies did not reveal noticeable grain growth in the specimen
(Fig. 3). The softening at low-temperature region may be a con-
sequence of reduction of dislocation density due to static recovery
and relaxation of internal residual stresses resulting from the an-
nihilation and rearrangement of dislocations. At higher tempera-
ture range (300–450 °C), a significant reduction of hardness is
observed with marginal increase in grain growth which may be
due over ageing effect (Fig. 4).
340 F. Khan MD, S.K. Panigrahi / Materials Science & Engineering A 675 (2016) 338–344
Fig. 2. TEM micrographs of FSPed UFG QE22 magnesium alloy. (FSP parameters-
Tool rotational speed in first pass: 800 rpm; Tool rotational speed in second pass:
600 rpm; Tool transverse speed: 100 mm/min).
3.2. Thermal stability of the FSPed UFG QE22 alloy
Fig. 6 shows the comparison of thermal stability of the present
work with various published literatures where different grade of
magnesium alloys were prepared via different SPD routes and then
subjected to annealing treatment of 60 min at different tempera-
ture regime. The primary observations made from Fig. 6 are: (i) the
microstructure of the FSPed QE22 magnesium alloy having grain
size 0.63 70.1 mm was thermally stable under UFG regime till
300 °C, whereas all other conventional magnesium alloys with
similar grain size shows faster grain growth at temperature lesser
than 200 °C. The authors in [16,21] developed grain sizes of
0.94 mm and 0.7 mm in a AZ31 alloy by two-step extrusion and
equal channel angular pressing (EXTþ ECAP) procedure and they
found that these UFG materials are thermally stable till 200 °C and
150 °C respectively. Matsubara et al. [20] obtained grain size of
0.7 mm in a Mg–9Al alloy by ECAP and found its thermal stability in
UFG regime till 200 °C. (ii) the average grain size of the present
FSPed QE22 magnesium alloy at annealing temperature of 450 °C
is measured as
3.8 mm (Fig. 5) which is significantly smaller than
other materials thermally treated under same condition. The grain
size obtained by Jain et al. in [14,15] at similar annealing condition
after FSP is found as 25 mm. (iii) abnormal grain growth was not
observed in the FSPed QE22 magnesium alloy (Fig. 3) in the whole
annealing temperature range of 100–450 °C; however this effect
was significantly observed in many other SPD materials above the
range of 150–200 °C [16,20,21].
Based on the above results and observations, the FSPed QE22
magnesium alloy shows excellent thermal stability in UFG regime
at high-temperatures. This is primarily due to pinning of thermally
stable eutectic Mg12Nd and Mg12Nd2Ag precipitates at grain
boundary which exerts strong forces to hinder the grain growth
called Zener drag pressure and also the influence the segregation
of RE solute Neodymium (Nd) atoms to grain boundaries which
retards the mobility of the grain boundaries by solute drag pres-
sure [36–39]. These two drag effects can be explained below.
3.3. Solute drag effect
Solute drag effect is the ability of the solutes to segregate along
the grain boundaries which has tendency to suppress the grain
growth by arresting the mobility of grain boundaries. In order to
overcome this, an additional drag pressure is required on the
boundaries. The drag effect depends on the depth of the free en-
ergy well associated with solute located on the grain boundary,
the diffusivity of the solute species and the boundary velocity.
Robson has demonstrated that a simple classical grain boundary
segregation and solute drag model (the Cahn–Lucke–Stuwe model
[4,40]) can be used to estimate the tendency of solute elements to
segregate at grain boundaries and to obtain the required drag. As
per their model the tendency for grain boundary segregation of
solute atoms can be calculated as per the following equation.
⎛ −∆Gseg ⎞
XGB = XM exp⎜ ⎟
⎝ RT ⎠ (1)
where XGB is the maximum solute concentration on the grain
boundary, XM is the average solute concentration, ΔGseg is free
energy of segregation, R is the universal gas constant and T is
annealing temperature.
The present material QE22 contains 0.4 at% of Nd which is a RE
element. The atomic radius of Nd (rNd) is 0.188 nm which is 34%
higher than that of magnesium matrix (rMg ¼0.14 nm). This sig-
nificant atomic mismatch (34%) increases the ΔGseg and hence the
driving force for grain boundary segregation (XGB) of Nd atoms is
increased; resulting in segregation of higher concentration of so-
lute atoms in the form of Nd solute clusters at grain boundary.
These segregated Nd atoms at grain boundaries retard grain
boundary mobility in QE22 magnesium alloy upto higher anneal-
ing temperatures with several orders of magnitude greater than
that obtained from conventional solutes by Al or Zn additions.
Therefore, Nd based solute drag effect is the primary cause for
obtaining maximum thermal stability in the present FSPed UFG
QE22 alloy among other conventional UFG magnesium alloys
processed by other SPD routes.
3.4. Zener pinning effect
This effect also plays a major role in retarding the grain growth
during annealing by imparting pinning effect from the thermally
stable Mg12Nd eutectics and fine nano scale Mg12Nd2Ag pre-
cipitates along the grain boundaries in the UFG QE22 alloy. The
driving pressure (P) for grain growth arises from the curvature of
the grain boundary and is given by
αγb
P=
D (2)
where γb is the grain boundary energy and α is a small geometric
constant. Grain growth will occur when the driving pressure P is
more than the Zener pinning pressure (Pz) given by
3 ⎛ fv γb ⎞
Pz = ⎜ ⎟
2⎝ r ⎠ (3)
where fv is the volume fraction of randomly distributed particles
and r is the radius of the particle [41,42]
At annealing temperatures upto 300 °C, the fv/r ratio is ob-
served to be large due to the presence of high volume fraction of
small Mg12Nd eutectics (o300 nm) and fine Mg12Nd2Ag pre-
cipitates (o 50 nm); which results higher Pz than driving force and
hence retards the grain growth. As the temperature increases
above 300 °C upto 450 °C, the kinetics of grain growth increases
but still is significantly lesser than other published literature for
different UFG magnesium alloys. In this range (i) the size of
 F. Khan MD, S.K. Panigrahi / Materials Science & Engineering A 675 (2016) 338–344 341

Fig. 3. Microstructure evolution of FSPed UFG QE22 magnesium alloy annealed for 60 min at different temperatures. (A) 100 °C ; (B) 200 °C; (C) 300 °C; (D) 400 °C.

Mg12Nd eutectics have coarsened from 300 nm (at 300 °C) to
850 nm (at 450 °C) and shaped in to round morphology shown in
Fig. 7 and (ii) evolution and partial growth of nano size Mg12Nd2Ag
precipitates occurred along the grain boundaries. Due to the pre-
sence of coarse Mg12Nd eutectic, there is a reduction in fv/r ratio
which weakens the Zener pinning pressure for retarding the grain
boundary migration and hence the tendency of grain growth in-
creases. But at critical size (r) of the eutectics both of the forces
equals (Pz ¼P) each other and hence resulted in partial increase in
grain growth even at high annealing temperature (450 °C). The
presence of nano Mg12Nd2Ag precipitates along grain boundary at
high-temperature domain lead to further retard grain boundary
migration.
In summary, the excellent thermal stability observed in UFG
QE22 alloy is due to simultaneous action of solute drag effect
because of segregation of Nd atoms along the grain boundaries
and strong Zener pinning effect due to uniform distribution of
both Mg12Nd eutectics and fine nano size Mg12Nd2Ag precipitates.
3.5. Grain growth kinetics
To study grain growth mechanisms during isochronal anneal-
ing it is necessary to determine the activation energy for grain
growth. Grain growth behavior in the investigated temperature
range was assumed to follow the general parabolic equation for
grain growth;
Dn − Don=kt (4)
Eq. (4) has the same form as Burke and Turnbull's equation
[43], where Do is the initial average grain size, D is the average
342 F. Khan MD, S.K. Panigrahi / Materials Science & Engineering A 675 (2016) 338–344
Fig. 4. Effect of annealing temperature on grain size, particle size and micro-
hardness of the FSPed UFG QE22 magnesium alloy.
Fig. 5. Microstructure of the FSPed QE22 magnesium alloy annealed at 450 °C for
1 h.
Fig. 6. Effect of annealing temperature on the grain size variation for FSPed QE22
magnesium alloy and compared with conventional magnesium alloys prepared via
different SPD processes. (FSP – Friction Stir processing; HR – Hot Rolling; ECAP –
Equal Channel Angular Pressing; ARB – Accumulated Rolled Bonding; EXT – Ex-
trusion; ACB – Accumulative Compression Bonding).
grain size at different annealing time t, n is the grain growth ex-
ponent and k is the grain growth constant which can be expressed
by Arrhenius equation;
Fig. 7. TEM microstructure of FSPed QE22 magnesium alloy at annealing treatment
of 450 °C for 1 h; showing round shaped morphology of eutectic Mg12Nd.
Fig. 8. Plot of ln(k) against 1000/T according to Arrhenius equation.
⎛ Q ⎞
k = k oexp⎜ − ⎟
⎝ RT ⎠ (5)
where ko is the pre-exponential term, Q is the activation energy, R
is universal gas constant and T is annealing temperature.
The grain growth exponent, n value is of primary importance
and it is a measure of the resistance to grain boundary motion in
the presence of impurity or alloying elements in solid solution. In
the ideal case (infinite crystal with no defects), the n should be
considered as 2. However, no material is ideal and hence “n” is
often found as above 2 due to various microstructural factor which
affects grain growth kinetics, such as compositional parameters,
the free surface effect, impurity-drag, solute drag, texture, dis-
location substructure and microstructure heterogeneities [32].
Higher values of n (in the range of 5–8) were observed mainly in
UFG magnesium and magnesium-based composites produced by
different SPD and mechanical alloying processes [17–19,30,31].
Therefore, in the present work, the activation energy is calculated
using two values of n as 5 and 8. Fig. 8 shows the plots made using
Arrhenius equation at different temperature domain of UFG QE22
alloy and than the activation energy was calculated using those
curves. It is found that the UFG QE22 alloy exhibits two different
grain growth mechanisms in two distinct temperature regimes
with different activation energies.
In the low-temperature range 100–300 °C, the activation en-
ergies are observed to be less than the grain boundary diffusion
(Qgb ¼ 92 kJ/mol) [22] of pure cast magnesium. The low activation
energy value in the low-temperature range may correspond to the
energy for stress relaxation process that results in reordering grain
boundaries and reducing the overall strain and energy of the
 F. Khan MD, S.K. Panigrahi / Materials Science & Engineering A 675 (2016) 338–344 343

Table 1
Comparison of activation energies of the present work with various SPD processed UFG magnesium alloys.

Material Process Grain growth exponent (n) Temperature (°C) Activation energy Q (kJ/mol) Reference

AZ31 HR 4 250  450 81 [18]

AZ31 ACB 5 350  450 105 [17]
AZ31 HP 5 300  400 110 [19]
QE22 FSP 5 300  450 180 Present work
Mg-Cu MA 7 300  400 118 [31]
Mg-Al Alloy MA 7 300  500 119 [30]
Mg-Al-Ti Alloy MA 8 300  500 123 [30]
QE22 FSP 8 300  450 280 Present Work

HR – Hot Rolling; ACB – Accumulative Compression Bonding; HP – Hot Pressing; FSP – Friction Stir processing; MA – Mechanical Alloying

materials without significantly losing the UFG structure. In the
high-temperature range 300–450 °C, the activation energies are
exceptionally higher than lattice self-diffusion (QL ¼135 kJ/mol) of
pure cast magnesium [44]. The comparative activation energies of
the present work with various SPD processed UFG magnesium
alloys have been represented in Table 1. The activation energies of
the present UFG QE22 alloy are observed to be significantly higher
than that of other SPD processed UFG magnesium alloys. The
higher activation energies achieved in UFG QE22 alloy could be
attributed to the following reasons; (i) retardation of grain growth
at elevated temperatures by uniform distribution of eutectic
Mg12Nd and pinning action of fine precipitates of Mg12Nd2Ag
along the grain boundaries. (ii) diffusivity of the alloying elements
Nd and silver (Ag) in magnesium is also one of the factor that
contributing to the high activation energy of the QE22 alloy. The
presence of RE element Nd and Ag in QE22 alloy has good affinity
with magnesium to form thermally stable Mg12Nd eutectic
(melting point 535 °C) and fine Mg12Nd2Ag precipitate which has
tendency to lower relative diffusivity at moderate temperatures
and good matrix coherency (iii) it has been discussed in the earlier
section that, in the present UFG material Nd solute atoms are
segregated along the grain boundaries which has strong tendency
in developing the weaker texture (non-basal texture) in magne-
sium by solute drag effect. Therefore it is expected to have a sig-
nificant effect on the mobility of both basal and non-basal slip
planes and hence the activation energies required for both basal
and non-basal slip systems can be increased by the solute drag
effect [8].
4. Conclusions
In summary developed UFG microstructure in QE22 alloy by
FSP has retained its microstructure in UFG regime at high-tem-
peratures till 300 °C. The activation energy and thermal stability of
the present UFG QE22 alloy was found to be higher than that for
other conventional UFG magnesium alloys processed by different
SPD routes. The strong pinning forces of thermally stable eutectic
Mg12Nd and fine precipitates Mg12Nd2Ag lying along the grain
boundaries and solute drag effect from the segregation of RE so-
lute atoms (Nd) at the grain boundaries in the FSPed UFG QE22
alloy provide contributing factors for high thermal stability and
activation energy at higher temperatures. This type of materials
which has extraordinary thermal stability is expected to behave
excellent superplastic formability due to grain boundary sliding
effect and hence the present material may find its suitable appli-
cations in forming and structural industries.
Acknowledgments
The authors gratefully acknowledge the financial supports from
ICSR-IITM, India through the grant number of MEE/12-13/584/
NFSC/SUSH.
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