Journal of Materials Science & Technology 50 (2020) 257–270

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Journal of Materials Science & Technology

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Research Article

Normal and abnormal grain growth in magnesium:

Experimental observations and simulations
Risheng Pei ∗ , Sandra Korte-Kerzel, Talal Al-Samman
Institut für Metallkunde und Materialphysik, RWTH Aachen University, D-52056, Aachen, Germany

a r t i c l e i n f o a b s t r a c t

Article history: Commercial purity as-cast magnesium was hot rolled and subsequently annealed at different tempera-
Received 23 June 2019 tures in order to investigate its grain growth behavior and link it to the texture evolution. Annealing at an
Received in revised form 19 August 2019 intermediate temperature of 220 ◦ C gave rise to abnormal grain growth with a few grains reaching a grain
Accepted 21 September 2019
diameter 10 times larger than the mean. Increasing the annealing temperatureto 350 ◦ C yielded normal
Available online 5 March 2020
grain growth. Both types of grain growth revealed a strengthening of the (0001) 11−20 texture compo-
 
Keywords: nent. It is hypothesized that a dislocation density gradient after recrystallization grants (0001) 11−20
Pure magnesium grains a size advantage during early stages of growth. The type of growth will be, however, determined
Grain growth by the mobility of the present grain boundaries and triple junction drag, which are strongly dependent
Texture on the annealing temperature. The above hypothesis of the interplay between these parameters was
Dislocation density gradient
explored through curvature- and residual dislocation-density-gradient-driven grain growth simulations
Level-set modeling
using a formerly developed level-set approach. The simulation outcome suggests that application of such
a modeling approach in microstructure studies of magnesium can provide valuable new insights into the
problem of grain growth and associated texture evolution.
© 2020 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science &
Technology.

1. Introduction
Grain growth (GG) behavior during thermomechanical treat-
ments plays a significant role in the investigation of metallic
materials owing to the close dependence of properties upon grain
size [1]. There are two types of grain growth: normal grain growth
(NGG) and abnormal grain growth (AGG). NGG takes place when the
average grain size continuously increases with the annealing time
and the grain size distribution remains self-similar, i.e. the shape
of the size distribution does not change [2]. By contrast, if AGG
occurs, the grain size distribution will vary significantly in terms of
height and width [2]. AGG is also termed secondary recrystalliza-
tion because only few grains grow rapidly and consume the rest of
the microstructure. As a result, a bimodal distribution of fine and
coarse grain sizes is typically observed during this process until it
completes and gives rise to a new unimodal distribution [1,2].
∗ Corresponding author.
E-mail addresses: pei@imm.rwth-aachen.de (R. Pei),
Korte-Kerzel@imm.rwth-aachen.de (S. Korte-Kerzel),
tasamman@imm.rwth-aachen.de (T. Al-Samman).
AGG has been widely reported in many metallic materials, e.g.
magnesium alloys [3,4], stainless steels [5], Fe-Si steel [6,7], tita-
nium alloys [8] and aluminum alloys [9,10]. However, its driving
mechanisms are still not entirely clear, and in some cases even con-
troversial. In the literature a variety of mechanisms were proposed
to explain this phenomenon, which are summarized as follows:
(i) Anisotropic grain boundary characteristics (i.e. mobility and
energy) of high and low angle boundaries, as pointed out by
Bhattacharyya et al. who studied the grain growth behavior of
a strongly textured AZ31B magnesium alloy [4].
(ii) Boundary pinning induced by solute and/or Zener drag, which
was for example reported by Basu et al. in their work on
rolled and annealed Mg-Gd and Mg-Dy alloys [3]. Interest-
ingly, they found that AGG occurred in Mg-Gd but not in Mg-Dy
alloy upon annealing at 450 ◦ C for 1 h. This was attributed to
the stronger grain boundary solute segregation effect shown
by Gd in comparison to Dy. As a consequence, at sufficiently
elevated annealing temperatures, grains with a topological
advantage would possess sufficient boundary velocities to
overcome solute drag and grow rapidly relative to other grains,
which would be eventually consumed due to their growth
restriction [3].

https://doi.org/10.1016/j.jmst.2020.01.014
1005-0302/© 2020 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science & Technology.
258 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270
(iii) Special, coincidence site lattice (CSL) boundaries, as in 13
(27.8◦ <0001 >) [11] and 11 (35.1◦ <0001>) [12] were also
highlighted in the context of selective growth in hexagonal
materials based on the premise of being low energy and high
mobility boundaries.
(iv) Solid-state wetting. The occurrence of AGG in Fe-Si alloys
was initially attributed to a grain size advantage neces-
sary to overcome the Zener pinning force [13–16]. However,
other studies argued that this theory cannot explain the phe-
nomenon because such size advantage was not always evident
after recrystallization [17–19]. Recently, solid-state wetting
was proposed to explain the preferential growth of grains
with {110}<001> GOSS orientation in Fe-3%Si alloy [7,20–23].
The basis of this theory stems from the concept of sub-
grain boundaries being low energy boundaries, which drives
their expansion at the expense of high angle boundaries with
a much higher energy [7,20–23]. Therefore, GOSS-oriented
grains, which are rich in low energy boundaries, exhibit pref-
erential growth over other grain orientations.
(v) Residual dislocation density gradients (DDG). In addition to
grain boundary curvature, differences in the remaining stored
dislocation energy among adjacent grains after recrystalliza-
tion provide additional driving force for grain boundary motion
during further annealing [24,25]. Boundaries of grains of lower
dislocation density will migrate faster than those that possess
a higher dislocation density in order to minimize the total free
energy of the system. This could eventually lead to AGG after
long-time annealing treatments.
(vi) Grain boundary complexion transition. This mechanism has
been widely reported for several different doped alumina sys-
tems [26,27], where AGG was associated with the presence of
certain grain boundaries that not only had higher mobility,
but also microscopically distinguishable structures and com-
positions, referred to as complexions [26,28,29]. Based on this,
complexions are found to promote AGG if transitions of a frac-
tion of grain boundaries dramatically increase their mobility
relative to the average surrounding grain population.
In the present study, we investigated the grain growth behavior
in Mg. For this, we used (commercially) pure Mg in order to sys-
tematically exclude several of the above-mentioned phenomena
related to the presence of alloying elements in order to improve
our understanding of the underlying mechanisms in Mg itself.
The material was hot rolled, recrystallization annealed and then
subjected to grain growth annealing treatments at different tem-
peratures for different times in order to quantitatively investigate
its grain growth behavior and the corresponding texture evolu-
tion. Interestingly, AGG was observed for annealing treatments at
a relatively low temperature of 220 ◦ C but not at higher tempera-
tures such as 350 ◦ C even after 7 days of annealing. With the use of
experimental characterization techniques combined with level-set
grain growth computer simulations, this work attempts to clarify
the mechanisms responsible for the aforementioned growth behav-
ior invoking several potentially important parameters that interact
differently at varying temperatures.
2. Experiments
2.1. Specimen processing
As-cast pure Mg (99.95%) was hot rolled at 400 ◦ C (nomi-
nal furnace temperature) from 15 mm to 1.2 mm by 7 passes
employing 30% thickness reduction per pass. Between the passes
the rolled specimen was returned into the furnace for 10 min to
regain the rolling temperature. The final pass was followed by
rapid water quenching. The rolled material was then subjected
to recrystallization annealing at 200 ◦ C for 1 h, followed also by
water quenching to freeze the obtained recrystallized microstruc-
ture. This step was quite challenging because the aim was to attain
full recrystallization without triggering grain growth. Therefore,
we chose a relatively low annealing temperature to have a bet-
ter control of the onset of grain growth, where we ended up with
almost a fully recrystallized structure, with the exception of a few
grains that remained unrecrystallized. The average grain size of
this microstructure was ∼15 ␮m, which served as the starting
microstructure for the following grain growth annealing experi-
ments, and as input for the simulations. For the grain growth study,
smaller samples were machined from the recrystallized state and
annealed at 220 ◦ C for 10 min, 30 min, 2 h, 8 h, 16 h, 24 h, 3 days
as well as 7 days. Additional annealing experiments at 350 ◦ C for 7
days were performed to study the long duration growth behavior
at a higher temperature.
2.2. Microstructure and texture characterization
Specimens for optical microscopy and electron back scatter
diffraction (EBSD) were prepared by grinding and mechanical pol-
ishing, followed by electro-polishing in an electrolyte of ethanol
and H3 PO4 (5:3), for 45 min at 2.00 V. For chemical etching a solu-
tion consisting of 10 ml H2 O, 10 ml CH3 COOH and 70 ml picral (4%
picric acid in a solution with ethanol) was used. The characteri-
zation of grain size and grain size distribution of specimens with
different annealing conditions was done by means of a Matlab code
based on the linear intercept method. LEO-1530 scanning electron
microscope (SEM) equipped with a field emission gun operated at
20 keV, and HKL Nordlys II EBSD detector was employed to carry
out the EBSD measurements. The EBSD data was analyzed and
visualized by the Matlab toolbox MTEX [30]. The macrotextures of
the investigated specimens were determined by X-ray pole figure
measurements using a Bruker D8 diffractometer equipped with a
high resolution area detector. To improve the grain statistics the
specimen was oscillated in the diffraction plane during the mea-
surement. Six incomplete pole figures, namely {10 1 0}, {0002},
{10 1 1}, {10 1 2}, {11 2 0} and {10 1 3}, were first measured using
filtered iron Fe-K˛ radiation at 30 kV and 25 mA. Then, the orienta-
tion density function (ODF) was determined and used to recalculate
the complete pole figures.
2.3. Computational procedure
For the simulation work in this study, a recently developed Grain
Growth Level Set simulation tool (GraGLeS) [31–33] was applied to
explore the effect of residual dislocation density gradients, remain-
ing in the microstructure after recrystallization, on the grain growth
behavior during further annealing treatments. This model, which is
available as an open source code [34], was chosen due to its excel-
lent computational stability and good description of the physics
of grain growth. This being its capability of considering a variety of
parameters influencing grain growth, such as anisotropic boundary
properties (if required), and finite triple junction mobilities. It also
allows for real-time-scaled simulations and can incorporate both
interface and volume energies as driving forces. The latest devel-
opment of this model featured a 3D approach tailored for parallel
computing [33]. In that study, the authors addressed a case of mag-
netically driven grain boundary motion in titanium incorporating
magnetic energy densities that are dependent on the grain orien-
tation with respect to the field direction. For general information
on the development of the level-set (LS) method as a determinis-
tic approach for modeling grain growth, the reader is referred to
[32,35–39].
 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270
For convenience, the following is a brief reproduction of some
of the information provided in [31–33] regarding the model setup.
Numerical details of the basic and new algorithm will not be
addressed here. The LS method is a mathematical framework to
describe interfaces and their evolution with time. Grain growth is
treated in this method as a competing shrinkage/growth of adja-
cent grains driven by a minimization of grain boundary energy,
where the topological transition and the extinction of entire grains
is automatically solved by means of Predictor-Corrector procedure.
This poses a true advantage over Vertex models since they require
explicit instructions to solve such transformations. The computa-
tional scheme of the basic LS algorithm consists of two main steps:
(i) Initialization of the input microstructure, where a signed distance
function (SDF) is assigned to each grain. This function repre-
sents both the entire grain and the grain boundary during the
evolution algorithm.
(ii) Computation of grain growth, where an iterative procedure of
three sequential steps is utilized to process the SDF of each
grain. (1) Predictor step that computes the motion of individual
grains by mean curvature flow of their interface. This motion
can be subsequently altered in order to consider interfacial
anisotropy effects. (2) Corrector step that restores the topo-
logical integrity of the microstructure by removing voids and
overlaps between neighboring grains. (3) Reinitialization step,
where the distance functions resulting from the corrector step
are computed to new interface positions.
The velocity (growth rate) of the migrating boundary at a specific
time t was calculated as:
dr
= = meff (k + pDDG ) , r = r0 for t = t0 (1)
dt
where meff denotes the effective mobility that takes into account
the mobility of triple junctions in addition to the boundary mobil-
ity, which can also influence the evolution of microstructure during
growth [32].  denotes the grain boundary energy, k the local cur-
vature of the grain boundary, pDDG the additional driving force
for grain growth resulting from orientation-dependent differences
in the residual dislocation density, remaining in grains after the
recrystallization annealing. Thus, during further annealing, recrys-
tallized grains with a lower residual dislocation density in their
environment will tend to consume other grains with a higher dis-
location density in order to minimize the total free energy. r is the
grain radius and r0 is the initial average grain size after recrystal-
lization. The dislocation density gradient (DDG) driving force was
introduced as:
pDDG = 0.5Gb2  (2)
where G is the shear modulus of pure Mg (16.7 GPa), b the Burg-
ers vector (0.321 nm for < a>-dislocations), and  the difference
in the residual dislocation density of adjacent grains of a certain
grain boundary. The estimation of  was based on experimental
EBSD misorientation maps providing information on the geomet-
rically necessary dislocation (GND) densities, and should therefore
be treated as an order of magnitude estimate, as discussed in Sec-
tion 4.2. The grain boundary energies were assumed to depend on
the misorientation angle  between adjacent grains according to
the Read-Shockley model [40].
  
      ally sufficient to induce AGG, yet only if combined with much longer
  = max ◦ 1-ln  ◦  , for  ≤ 15◦
 (3)
15 15
The energy of high-angle grain boundaries ( ≥ 15◦ ) was con-
sidered constant;  (15◦ ) = max = 0.5 J/m2 . Similarly, the mobility
of grain boundaries was considered to be exclusively a function of
the misorientation angle, where there was also a clear distinction
259
between the more mobile high-angle and the virtually immobile
low-angle boundaries.
  9 
  
  
m  = mmax 1-0.99exp −5  , for  ≤ 15◦ (4)
 15◦ 
In the absence of reliable mobility data for pure magnesium,
the mobility of general high-angle boundaries mmax was assigned
an estimated value of 4 · 10−14 m4 /Js for 0.53 Tm (220 ◦ C), and
4 · 10−13 m4 /Js for 0.67 Tm (350 ◦ C) on the basis of a study by
Okrutny et al. [41] dealing with modeling of static recrystallization
in AZ31 magnesium alloy. There, the authors extracted mobility
values by fitting experimental grain growth kinetics obtained at
different elevated temperatures to Hillert’s grain growth model.
Although we should be careful with the aforementioned mobil-
ity values, we note that their magnitude is not likely to affect the
overall growth trends (abnormal vs. normal growth) but rather the
temporal rate of growth in the simulated microstructures.
With respect to Eqs. (3) and (4), it is noted that these general-
ized approaches do not capture any special conditions that apply,
for example, to coincident site lattice boundaries or to cases where
Zener/solute drag necessitates the implementation of anisotropic
high-angle boundary energy or mobility. Another limitation of the
above equations is that they do not account for a possible depen-
dency of the boundary energy and mobility on the grain boundary
plane. Despite the fact that the model at our disposal is capable of
dealing with anisotropy effects to quantitatively model the rela-
tionship between grain growth and texture in magnesium alloys
(e.g. Basu et al. in [3]), it will be shown later that the simplified
assumptions regarding the mobility and energy of grain boundaries
work relatively well in reaching a satisfying agreement between
experimental microstructures and textures and their simulated
counterparts.
3. Results
3.1. Grain growth microstructures at 220 ◦ C and 350 ◦ C
The microstructures of pure Mg annealed at 220 ◦ C for different
times are shown in Fig. 1. It is obvious that after 8 h of annealing
there are a few large grains surrounded by a much higher pro-
portion of fine grains. Such configurations of large and fine grains
remained in the microstructure also for increased annealing times.
Additional annealing for 7 days at the same temperature (220 ◦ C)
was conducted to investigate whether AGG comes to completion or
whether a bimodal microstructure would still exist. Fig. 2 shows the
respective optical microstructure for a large representative surface
area of 10 × 8 mm2 . As evident, there was still a bimodal distribu-
tion relating to two groups of rapidly and slowly growing grains.
The average size of small grains remained at ∼ 40 ␮m and that of
the very coarse grains at ∼ 400 ␮m, namely, ten times larger.
In comparison to recent reports on AGG in Mg alloys, the 220 ◦ C
temperature used in the present study was markedly lower than
the temperatures used to trigger AGG in the literature [3,4,42].
The results of Wu et al. [42] and Basu et al. [3] showed that AGG
was evident in a magnesium-rare earth (Mg-RE) alloy containing
gadolinium, when deformed specimens were annealed at 450 ◦ C
– 500 ◦ C for 60 min – 80 min, respectively. For commercial AZ31
alloys, annealing temperatures between 300 ◦ C and 450 ◦ C are usu-
durations [4]. Therefore, in order to correlate the examined AGG
behavior in pure Mg with that reported for Mg alloys, an additional
set of annealing experiments was carried out at 350 ◦ C. Fig. 3 shows
an optical image after annealing at 350 ◦ C for 7 days. The size of
the observed area was 10 × 6 mm2 (Fig. 3(a)). It is evident from
the high magnification images (Fig. 3(b–d)), that the microstruc-
260 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270

Fig. 1. Optical microstructures of rolled and recrystallized specimens annealed at 220 ◦ C for different times: (a) – (d) representative micrographs at low magnification; (e) –
(h) specific areas of interest at high magnification.

Fig. 2. Optical microstructure of the specimen annealed at 220 ◦ C for 7 days: (a) Panoramic image of the whole sample area (10 × 8 mm2 ) (RD-TD plane); (b) – (d) magnified
images of several outlined areas in (a) revealing more details with respect to a few abnormally grown grains with an overwhelming size advantage compared to the rest of
the microstructure.
 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270
Fig. 3. Optical microstructure of the specimen annealed at 350 ◦ C for 7 days (analogous to Fig. 2): (a) Panoramic image of the whole sample area (10 × 6 mm2 ) (RD-TD plane);
(b) – (d) magnified images of several outlined areas in (a) revealing a more uniform grain size distribution than that in Fig. 2, which is taken as an indication for the absence
of AGG at 350 ◦ C.
ture with respect to the size distribution was much more uniform
in comparison to the 220 ◦ C case, i.e. there were no grains with an
overwhelming size advantage. This indicates that grain growth was
initiated globally, which led to NGG.
3.2. Grain boundary misorientation analysis
To examine the role of boundary misorientation in the occur-
rence of AGG, EBSD measurements were carried out on the
specimen annealed at 220 ◦ C for 7 days. The results are shown
in Fig. 4 in terms of inverse pole figures (IPF) and misori-
entation axis/angle distributions. As shown in Fig. 4(a), eight
abnormally-grown grains were marked with letters A to H, and
their misorientation data with respect to their direct fine-grained
neighbors (199 grain boundaries in total) was analyzed, as shown
in Fig. 4(c). For visualizing the distribution of misorientations axes
of the selected boundaries, the full circle of all twelve unit tri-
angles was used to quantify frequent misorientation axes that
could potentially identify special orientation relationships. The
corresponding colorbar represents the frequency of the plotted
misorientations. For example, if a specific misorientation axis
appears five times in the sampled data, it will be assigned the color
‘yellow’. Misorientation axes appearing one time only will be ‘dark
blue’ according to the color bar. In addition to the misorientation
axis distribution the boundary misorientation angle distribution is
also shown. From the data, approximately 10% (20out of 199)  of the
plotted misorientation axes corresponded to the 52−7−3 direc-
tion. The distribution of misorientation angles revealed a distinct
peak at 30◦ . Extended analysis included replotting all measured
261
misorientation axes in a single unit triangle and calculating
 the
rotation angles between the most common 52−7−3 axis and all
other axes. Theresults are
 plotted in the bottom part of Fig. 4(c).
As shown, the 52−7−3 misorientation axis was mostly related
to the other misorientation axes by rotations of ≤ 20◦ .
Analogous to the misorientation analysis of the abnormal grains
A–H, fine grains within a chosen area in Fig. 4(b) were also studied
(685 grain boundaries). Similarly, the distribution of the sampled
misorientation axes was more or less uniform within the unit tri-
angle. Almost
 10% of the misorientation axes were clustered about
52−7−3 . Additionally, certain misorientation axes on the arc
   
between 11−20 and 10−10 were also common with frequen-
cies between 5% and 8%. The misorientation angle distribution of
the fine grains did not show a single distinct peak at 30◦ but rather a
broad peak between 20◦ and 30◦ . In terms
 of special
 boundaries, the
misorientation relationship of 29.9◦ 11−20 found for an appre-
ciable proportion of grain boundaries in Fig. 4 does correspond to
a 15a CSL boundary for c/a=1.620 [11,43]. As this is a minimum-
energy, and not necessarily a high mobility boundary, its stability
during grain growth is reasonable.
3.3. Texture analysis
It is reported in the literature that few grains with specific orien-
tations can grow to abnormal sizes, as for example in a Fe-3%Si alloy.
In such material, grains with a GOSS orientation tend to grow faster
than others [6,7,20–23]. In this work, to evaluate the orientation of
abnormally large and small grains, the microstructure of the speci-
men annealed at 220 ◦ C for 7 days was divided into two grain groups
262 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270

Fig. 4. Grain boundary misorientation analysis results of the microstructure annealed at 220 ◦ C for 7 days: (a) ND-IPF map of the sampled area containing both very large and
small grains (step size: 2 ␮m, area: 1600 × 1200 ␮m2 , mean MAD: 0.61◦ ). Blue and white boundaries denote high and low angle boundaries (<15◦ ); (b) selected area from
(a) with only small grains; (c) and (d) misorientation axis and angle distributions of grain boundaries of very large and small grains, respectively. The color coding denotes
the frequency of plotted misorientation axes in the unit triangles.

using a cutoff with respect to the average grain size in the analyzed
EBSD map (33.9 ␮m). When the grain area was more than four times
larger than the average one, the respective grain was assumed to
be a large grain. The analysis is shown in Fig. 5(a) and (b) in terms
of IPF-coloring maps with reference to the rolling direction  (RD).
Most of the very large grains were colored green ( 11−20 RD),
whereas the small grains
 were highlighted
 in both green and blue
exhibiting both 11−20 RD and 10−10 RD orientations. Cor-
respondingly, the basal and prismatic pole figures were plotted for
both datasets to locate the position of maximum basal and pris-
matic pole density. A comparison of the basal pole figures showed
that the basal poles were very closely aligned with ND but the tex-
ture strength was different. Obviously, the few large grains dictated
the measured sharp basal texture. Interestingly, when compar-
between small grains) are separated by 30◦ , which correlates well
with the findings in Fig. 4 with respect to the misorientation angle
distribution. The resultcould also suggest that in this particular
case the (0001) 11−20 orientation bears a certain growth advan-
tage among other basal-oriented grains. In order to validate such
growth advantage statistically, another two EBSD maps were per-
formed and altogether more than 8000 grains were indexed. The
corresponding pole figures of large and small grains are shown in
Fig. 5(c) and (d), and intensities along the outmost circle (˛ = 90◦ )
on (11 −2 0) plane with ˇ increased are plotted in Fig. 5(e). Both of
the pole figures and intensity  distributions confirmed the growth
advantage of (0001) 11−20 orientated grains.
The macrotextures of the specimens annealed at 220 ◦ C and 350
◦ C for 16 h and 7 days are given in Fig. 6. In comparison to the fully

 polefigures (either one) the very large grains

ing the prismatic recrystallized (initial) state, the bulk texture did not change dur-
were of (0001) 11−20 orientation, and the small grains of (0001) ing the annealing treatments at 220 ◦ C regardless of the annealing
 
10−10 orientation. These two orientations (which coexist also duration (Fig. 6(a–c)). The growth advantage seen in the EBSD data
 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270 263

Fig. 5. Grain orientation analysis results (220 ◦ C / 7 days) for very large grains and small grains in terms of RD-IPF maps (a) and (b) along with the corresponding basal and
prismatic pole figures; (c) and (d) pole figures of large and small grains of more than 8000 grains gotten by multi-EBSD measurements; (e) intensity on (11 −2 0) plane along
the outmost circle (˛ = 90◦ ) with angle ˇ increased. Texture intensity is given in terms of multiples of a random distribution.

for the annealing condition of 220 ◦ C / 7 days was not visible in
the XRD data. At 350 ◦ C and after 7 days ofannealing, there was an
obvious strengthening of a (0001) 11−20 type texture, where the
 
11−20 directions became strongly aligned with the RD (Fig. 6(d)).
4. Discussion
To summarize the results reported above, a very different grain
growth behavior was observed upon annealing of hot rolled, com-
mercially pure magnesium at 220 ◦ C (AGG) and 350 ◦ C (NGG) for
long times up to 7 days. Texture analysis revealedindications
 of
a certain growth advantage for basal grains with 11−20 || RD
orientation. Boundary misorientation analysis of a microstructure
comprising the two grain groups of the very large and the much
◦
 a frequent
smaller ones revealed  misorientation angle of 30 and
misorientation axis 52−7−3 associated with the very large grains
and their direct neighbors. This section discusses the mechanisms
that could explain the rather unexpected occurrence of abnormal
grain growth in deformed pure magnesium at certain annealing
conditions, where a size advantage would not be a sufficient rea-
son for the overwhelming growth of a few grains at the expense
264 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270
Fig. 6. XRD bulk textures of selected specimens: (a) as-recrystallized; (b) annealed at 220 ◦ C for 16 h; (c) annealed at 220 ◦ C for 7 days; (d) annealed at 350 ◦ C for 7 days.
Texture intensity is given in terms of multiples of a random distribution.
of other much finer grains. The discussion presented is supported
by level set computer simulations of grain growth, implementing
anisotropic microstructural conditions, such as different bound-
ary mobility, triple junction drag and different densities of stored
dislocations after recrystallization.
4.1. Possible mechanisms for the occurrence of AGG in pure
magnesium
The driving force for grain growth is the minimization of the
grain boundary energy, which greatly contributes to the reduc-
tion of the total free energy of the system [1]. During grain growth,
grains merge in order to decrease the total grain boundary area. This
process can give rise to an initial size advantage for some grains,
so that they grow faster at the expense of smaller neighboring
grains [44]. However, this cannot explain why  in some
 particular
cases only a few grains, mostly with (0001) 11−20 orientation,
were seen to preferentially grow to overwhelming sizes. The ini-
tial recrystallized microstructures of such cases do not show any
obvious peculiarity with respect to orientation, grain size or grain
orientation spread (GOS) distributions. An example is shown in
Fig. 7 of a sample subjected to recrystallization annealing at 200
◦ C for 1 h. The EBSD maps in Fig. 7(a) and (b) show the orientation
of recrystallized grains with respect to RD, and the correspond-
ing GOS values, respectively. To quantitatively assess the role of
grain size and size distribution in selecting texture components, the
recrystallized grains (GOS < 1) shown in Fig. 7(a) were categorized
   
into either (0001) 11−20 or (0001) 10−10 groups based on
the smallest rotation to reach either orientation. The correspond-
ing size distributions in terms of grain number and area fractions
are plotted
 in Fig. 7(c)  and (d),
 respectively. Evidently, the (0001)
11−20 and (0001) 10−10 oriented grains exhibit almost iden-
tical distributions for the whole range of grain sizes measured. This
is important
 because it proves that the larger grains in the (0001)
11−20 texture during AGG at 220 ◦ C (Fig. 5) do not originate from

the recrystallized condition.  also applies to the global strength-
This
ening of the (0001) 11−20 component during NGG at 350 ◦ C,

which cannot be attributed to an initial size advantage in the (0001)
11−20 distribution present in the recrystallized condition.
From Eq. (1), the driving force for grain growth is directly pro-
portional to the grain boundary energy and the boundary curvature.
If the microstructure comprises a certain proportion of special low
energy boundaries, the characteristics of grain growth could exhibit
an anisotropic behavior. Although we have seen some indications of
CSL grain boundaries in the microstructures of our annealed spec-
imens, we cannot claim with confidence that this mechanism is
the main driver for the AGG behavior reported here. Due to their
lower energy, it is not unreasonable to assume that CSL boundaries
can survive long duration annealing treatments, and thus remain
in the microstructure. From the perspective of anisotropic bound-
ary properties, different relative mobility values could potentially
lead to an abnormal growth behavior. When the movement of grain
boundaries is restricted by some factors, like solute or Zener drag
resulting from boundary interaction with solute atoms or precipi-
 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270
Fig. 7. Initial microstructure of the recrystallized condition at 200 ◦ C for 1 h prior to grain growth 
size: 1.5 ␮m, area: 1800 × 1500 ␮m2 , mean MAD: 0.68◦ ); (b) GOS map up to 5◦ . (c) & (d) (0001) 11−20 and (0001) 10−10 size distributions of GOS <1◦ grains depicted
in terms of grain number and area fractions.
tates, AGG can occur. This was for example reported by Basu et al. [3]
who investigated the effect of solute segregation to grain bound-
aries on the grain growth behavior and resulting weak textures
in magnesium-rare earth alloys. They attributed the occurrence of
AGG in Mg-Gd alloy to the hypothesis that at a sufficient annealing
temperature some grain boundaries are able to overcome the pin-
ning effect and grow to larger sizes compared to other boundaries
that remain pinned. Having used pure magnesium in the current
study, the pinning mechanism does not offer a suitable explana-
tion for the occurrence of AGG. It is noted that the material still has
impurities but we believe their concentration is too low to induce
significant pinning effects. After all, solute or Zener drag should
not be dependent on the  grain orientation
 since it was mostly the
grains with the (0001) 11−20 orientation that seemed to grow
abnormally.
Another mechanism that has been proposed to understand the
occurrence of AGG in Fe-Si alloys is the so-called solid-state wet-
ting. The theoretical description of this mechanism can be found
in [45,46], whereas Fig. 8 schematically illustrates its basic prin-
ciple. The numbers associated with the grain boundaries denote
their energies. The sum of energy of grain boundary AA* and grain
boundary BA* is smaller than the energy of grain boundary AB so
that the boundaries AA* and BA* tend to expand at the expense of
the boundary AB. This means that grain A* will grow and eventu-
ally consume grain A, as illustrated in Fig. 8(a) [47]. Based on the
same principle of energy minimization, a different case is shown, in
265
 annealing
 presented
treatments  in terms of (a) RD-IPF EBSD map (step
Fig. 8(b), where grain A grows at the expense of grain A* [47]. It was
found that this mechanism necessitates the presence of some low
energy boundaries, such as sub-grain boundaries, which enhance
solid-stated wetting conditions around triple junctions. An exam-
ple of this is found for grains with GOSS orientation in silicon steel
[7,21,47].
From the above, it is thus to be expected that as a consequence
of grain growth driven by solid-state wetting, the fraction of sub-
grain boundaries should increase in the annealed microstructures
[23,48]. However, as for our data, a comparison of the misorienta-
tion angle distributions (␪ ≤ 15◦ ) for as-recrystallized specimens
(initial state) and those annealed at 220 ◦ C for 7 days (final state)
revealed no significant variation (Fig. 9). According to Shim et al.
[20], low energy boundaries are frequently found in silicon steel
annealed microstructures because the GOSS-oriented grains, which
typically have a lower stored energy after deformation, rather
recover than recrystallize. In our material, due to the small varia-
tion in the texture, it is not likely that some grain orientations only
undergo recovery while other orientations undergo recrystalliza-
tion. This would eliminate the possibility of having a considerable
fraction of remnant sub-grain boundaries after recrystallization
that is sufficient to trigger solid-state wetting during further grain
growth annealing treatments.
From another perspective, it might be possible that  the differ-

ent fiber components of the basal texture, i.e. (0001) 11−20 and
 
(0001) 10−10 , have some variations in their remaining stored
266 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270

Fig. 8. Schematic illustration of the solid-state wetting mechanism of grain growth in silicon steel reproduced from [47]. The numbers at the grain boundaries denote
examples of their energies.

Fig. 9. Comparison of the fraction of low angle boundaries (up to 15◦ ) present in (a) the initial recrystallized condition, and (b) in the annealed condition at 220 ◦ C for 7 days.

energy upon recrystallization (even though it is much lower) that
could influence their grain growth behavior based on the DDG
mechanism described earlier in the context of possible AGG drivers.
 Zhu etal. reported
In fact, in a relevant study of a Zr-2Hf alloy [12],
a favorable increase in the intensity of the 11−20 fiber over
 
the 10−10 fiber during primary recrystallization and normal
grain growth. In the current case, when recrystallized specimens
are annealed at low temperature (220 ◦ C), stored dislocations are
not likely to have enough energy to move and are thus  trapped

inside grains. From the discussion above, grains with 11−20 ||
 
RD and 10−10 || RD orientations are likely to exhibit a gradi-
ent in their residual dislocation density,producing
 a driving force
for a selective grain growth to consume 10−10 grains and elim-
inate their higher dislocation density. Moreover, in addition to
the DDGinduced driving force, a resulting grain size advantage of
11−20 grains could also accelerate their further growth, while
the other grains remain comparably small because of relatively
low grain boundary mobility and high  triple  junction drag at the
this temperature. Eventually, such 11−20 grains would evolve
into abnormally grown grains with much larger sizes than the sur-
rounding grains. In this scenario, AGG will cease when the very
large grains come to impingement. Note that in the experiments
reported above, the corresponding XRD bulk texture did not change
too much in comparison to the recrystallized texture (Fig. 6(b) and
(c)), which can be related to the small fraction of abnormally grown
grains in the annealed microstructure at 220 ◦ C. It is noted that the
average grain size in this case remained below 50 ␮m.
On the other hand, when the specimens are annealed at a higher
temperature (350 ◦ C), dislocations trapped inside grains can be
expected to be more mobile and thereby be easily absorbed by their
nearest grain boundaries decreasing the anisotropic nature of grain
growth arising from DDG. In addition, thermal activation by rais-
ing the temperature is also expected to drastically decrease the
triple junction drag [49] and increase the grain boundary mobil-
 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270
Fig. 10. Schematic illustration for abnormal and normal grain growth occurring in annealed pure magnesium at 220 ◦ C and 350 ◦ C, respectively. The length and the thickness
of the arrowsrepresent
 the magnitude of the impact of boundary mobility and DDG at each temperature. The number of G2 grains was restricted to those with almost an
ideal (0001) 11−20 orientation (c.f. Section 4.2).
ity. As aresult, the difference in the growth rate between (0001)
11−20 grains and their neighbors should decrease, preventing
the occurrence of AGG. With respect to texture evolution, there was
 basal texture and a
a significant strengthening of the recrystallized
clear transition from a basal fiber to a (0001) 11−20 component
(Fig. 6(d)). This is likely to emanate from a remaining DDG effect
that provides grains of that orientation with an advantage during
growth. Fig. 10 provides a schematic illustration of the two cases
discussed above with the conditions that lead to AGG and NGG at
220 ◦ C and 350 ◦ C, respectively.
4.2. Level-Set computer simulations of grain growth
The hypothesized roles of local dislocation density, triple junc-
tion drag and grain boundary mobility for the specific texture and
grain size distributions found in the experiments, can be inves-
tigated further by Level-Set simulations that allow systematic
variation of each parameter.
Initial microstructures for the simulation were obtained by EBSD
measurements after recrystallization annealing at 200 ◦ C for 1 h
(Fig. 7). As shown in Fig. 7, the recrystallized microstructure can
be firstly divided into two grain groups based on their GOS values.
Grains with GOS>1◦ (group1, hereafter G1) are assumed to be recov-
ered, whereas grains with GOS<1◦ are considered recrystallized.
Although we did not employ high-resolution diffraction measure-
ments to estimate the stored energy in different grain groups,
we can reasonably assume that G1 grains are associated with a
267
higher residual stored energy than recrystallized grains. Among
the group of recrystallized
 grains we further distinguished between
(0001) 11−20 grains (G2) having a competitive advantage dur-
ing growthand all other
 recrystallized grains (G3). The selection of
the (0001) 11−20 grains was based on a criterion of maximum 5◦
◦
angle between the c-axis and ND and maximum 3 angle between
the 11−20 axis and RD.
The next step in the approach was to derive a rough estima-
tion of the dislocation density of the aforementioned three grain
groups. Stored dislocations in the material after annealing consist
of geometrically necessary dislocations (GNDs), which are typically
immobile, and therefore less prone to rearrangement and annihi-
lation events during recovery [50]. Unlike GNDs, which are formed
to account for lattice curvature during deformation, statistically
stored dislocations (SSDs) originating from statistical dislocation
entanglements [51] can undergo recovery resulting in reduction of
their density in the annealed microstructure [1]. In this work, the
kernel average misorientation (KAM) function was used to esti-
mate the GND densities for G1, G2 and G3 grains. Details of this
calculation method can be found in [52,53]. It is noted that the stan-
dard EBSD employed for the local orientation measurements has
an angular error of 0.5◦ -1◦ , which is thought to result in artificially
high GND densities, particularly in a recrystallized material with a
low total dislocation density. Our calculations, which are therefore
likely to be an overestimate, showed that the average GND densities
in the aforementioned three groups of grains were 1 × 1013 /m2 , 6
× 1012 /m2 and 9 × 1012 /m2 , respectively. Since it was not possible
268 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270

Fig. 11. Simulated grain growth microstructures and their corresponding textures at different time increments matching the experimental annealing times employed. (a, f)
input EBSD microstructure; (b - e) anomalous grain growth behavior equivalent to annealing at 220 ◦ C; (g – j) uniform grain growth equivalent to annealing at 350 ◦ C. The
color of grain boundaries denotes their relative mobility (red is maximum, purple is minimum).

to know the relation between the GND density and total disloca-
tion density, the latter was assumed to be 10 times larger than the
estimated GND density at 220 ◦ C. Hence, for the simulations at 220
◦ C, the total dislocation density in G1, G2 and G3 was taken as 1.0 ×
1014 /m2 , 6 × 1013 /m2 and 9 × 1013 /m2 , respectively. To incorpo-
rate the role of temperature in the simulations, the values assigned
to the dislocation densities, triple junction drag and grain bound-
350 ◦ C. In Fig. 11(b)–(e) some grains start to develop a significant
size advantage and proceed by eclipsing their neighboring grains,
resulting in a heterogeneous microstructure with very large and
very small grains. In Fig. 11(g)–(j) the simulations show a uniform
growth behavior with increasing annealing time. With respect to
texture, the simulated microstructures at different time steps were
exported back into the file format of the EBSD data used to pop-
ary mobility were adjusted according to the trends shown in Fig. 10.
For the 350 ◦ C case, the density of residual stored dislocations was
one tenth of that used in the simulations of the 220 ◦ C case, which
should be treated as an order of magnitude estimate. The bound-
ary mobility was increased by a factor of 10 and the triple junction
drag effect decreased by a factor of 1.3. These values showed a good
qualitative agreement with the target textures and microstructures
(grain size distributions) obtained from experiments.
Grain growth simulation results of evolved microstructure and
texture at 220 ◦ C and 350 ◦ C are displayed in Fig. 11 for different
time steps matching the experimental annealing times based upon
a similar average grain size to the one obtained in the experiments.
The different colors assigned to grain boundaries denote their rel-
ative mobility, with ‘red’ corresponding to maximum and ‘purple’
to minimum levels. The input EBSD microstructure with its unique
set of measured Euler angles is shown in Fig. 11(a) and (f). In both
cases of grain growth, the level set method, with the assumptions
made for each regarding the dislocation density gradient, triple
junction drag and boundary mobility was able to reproduce a very
similar growth behavior observed experimentally at 220 ◦ C and
ulate the simulations, which allowed for further texture 
analysis
using the MTEX software. The reproduced basal and 11−20 pris-
 figures
matic pole  in Fig. 11 show a gradual strengthening of the
(0001) 11−20 component with increasing annealing time. This
qualitative trend is in line with the experimental XRD and EBSD
measurements (Figs. 5 and 6). In terms of a quantitative agreement,
it was difficult to obtain comparable texture intensities due to the
limited number of remaining grains in the simulations at advanced
time steps, particularly in the case of NGG that would of course lead
to overstrengthening of the texture.
Fig. 12 presents a quantitative analysis of the simulation results
shown in Fig. 11. Fig. 12(a) shows a comparison of the temporal
grain size evolution for the two cases corresponding to 220 ◦ C and
350 ◦ C. For determining the grain growth behavior, i.e. distinguish-
ing normal from abnormal growth, different criteria can be used.
The most popular ones are based upon appearance of a bimodal
grain size distribution or variation in the breadth of the normalized
grain size distribution (loss of self-similarity) [2,4]. However, due
to the limited number of grains in the present simulations, we used
another method instead, which examines the ratio D/<d>, where D
 R. Pei et al. / Journal of Materials Science & Technology 50 (2020) 257–270
Fig. 12. Quantitative analysis of the simulated growth behavior shown in Fig. 11. (a) temporal grain size evolution for the two cases corresponding to 220 ◦ C and 350 ◦ C; (b)
variation of D/<d> with time; (c) variation of the derivative of D/<d> with time. D is the diameter of the largest grain and <d> is the average grain diameter of all grains.
is the diameter of the largest grain and <d> is the average grain
diameter of all grains [5,21,47,54–56]. Fig. 12(b) shows the tempo-
ral evolution of D/<d> for the two cases resembling annealing at 220
◦ C and 350 ◦ C. During the first 50 min, the initial D/<d> ratio does
not exhibit a strong variation, which is thought to be a period in
which the group of large recovered grains (G1) are eaten up by the
recrystallized grains due to their different stored dislocation den-
sities. This process would slightly decrease the D/<d> ratio. After
50 min of annealing (the beginning of the second period) the two
cases reveal a completely different evolution of D/<d> with increas-
ing annealing time. For the 220 ◦ C case, the D/<d> ratio increases
up to 12, while the D/<d> ratio for the 350 ◦ C case drops to 4. A
large D/<d> ratio indicates presence of island grains with a grain
size D many times larger than the average grain size <d>, which is
in turn indicative of anomalous growth. Thus, analogously, a small
ratio of D/<d> is characteristic for normal grain growth. For vali-
dation purposes, the experimental D/<d> data at 220 ◦ C was also
plotted in Fig. 12(b), which reveals a similar trend to attain high
values during period 2 annealing that spans between 50 min and 7
days. In a similar fashion to Fig. 12(b), (c) now presents a compari-
son of the derivative of D/<d>. This analysis considers the changes in
D/<d> that take place during successive time increments. A positive
derivative of D/<d> is used as in indicator of AGG, which is observed
for the simulated and experimentally obtained data at 220 ◦ C (inset
in Fig. 12(c)). The inflection point in the positive regime of AGG can
be interpreted as the impingement of the anomalously large grains
and resumption of NGG. Eventually, a steady state is reached after
very long annealing times, where D/<d> becomes constant.
5. Conclusions
In this work, commercial purity Mg was hot rolled and subse-
quently annealed at different temperatures for different times in
order to investigate its normal and abnormal grain growth behav-
ior and link it to the corresponding texture evolution. The following
main conclusions are parsed from the findings obtained by exper-
imental microstructure characterization and level set computer
simulations of grain growth.
(1) Annealing at an intermediate temperature of 220 ◦ C gave rise to
abnormal grain growth with a few grains having a grain diam-
eter 10 times larger than the average. Increasing the annealing
temperature to 350 ◦ C yielded normal grain growth.
(2) 
For both types of grain growth, strengthening of the (0001)
11−20 texture component was coupled with a competitive
growth advantage for grains with that orientation.  
(3) It is hypothesized that the fast growth rate of (0001) 11−20
grains is a result of gradients in the residual dislocation density
269
stored in grains after recrystallization. Other potential mecha-
nisms, such as special boundary misorientation relationships,
initial size advantage emerging from recrystallization, solid-state
wetting effects were discussed and considered less likely to play
an important role in the present case.
 force
(4) The driving  induced by a dislocation density gradient grants
(0001) 11−20 grains a size advantage during early stages of
growth. The type of growth will be, however, dictated by the
present grain boundary mobility and triple junction drag, which
are highly dependent on the annealing temperature.

(5) For annealing 
conditions where the temperature is low enough,
(0001) 11−20 grains would thus have a higher chance of rapid
growth and becoming abnormally large, while most of the other
grains grow at a much slower rate and remain comparably small.
This is due to a generally low boundary mobility and high triple
junction drag at low temperatures, where abnormal grain growth
occurs because normal grain growth is globally restricted. At a
much higher annealing temperature, the anisotropic nature of
grain growth arising from orientation-dependent density gradi-
ents will be extenuated because the residual dislocations inside
grains are more likely to be mobile and be absorbed by their sur-
rounding grain boundaries. Additionally, growth conditions will
be globally enhanced by an increase in the average boundary
mobility and a reduction of triple junction drag. This will lead
to normal grain growth.
(6) The above hypothesis of the interplay between dislocation
density gradient, boundary mobility, triple junction drag and
annealing temperature was explored through level set model-
ing of grain growth incorporating those aspects. The simulation
outcome reproduced the same trends for the normal and abnor-

mal grain growth occurring at the two investigated temperatures, 
including the characteristic strengthening of the (0001) 11−20
component. This suggests that application of this modeling
approach in microstructure studies of magnesium alloys can pro-
vide valuable new insights into the problem of grain growth and
associated texture evolution.
Acknowledgement
R.S Pei is grateful for financial support from the Chinese Schol-
arship Council (CSC).
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