Materials Science and Engineering A 528 (2011) 4239–4247

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Materials Science and Engineering A

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Particle effects on recrystallization in magnesium–manganese alloys:

Particle pinning
J.D. Robson a,∗ , D.T. Henry a,1 , B. Davis b
a
Manchester Materials Science Centre, Grosvenor Street, Manchester M1 7HS, UK
b
Magnesium Elektron North America, 1001 College Street, P.O. Box 258, Madison, IL 62060, USA

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

Article history: Dispersoid particles are widely used in wrought aluminium alloys to control grain structure dur-
Received 17 December 2010 ing thermomechanical processing. The aim of this work was to investigate whether this approach
Received in revised form 9 February 2011 could be utilized in wrought magnesium alloys to obtain better control of recrystallization. A binary
Accepted 9 February 2011
magnesium–manganese alloy was heat treated to produce a fine dispersion of manganese precipitates.
Available online 17 February 2011
The effect of this dispersion on dynamic and static recrystallization during channel die deformation (at
a slow strain rate), hot rolling, and annealing was studied and compared with that of an alloy free of
Keywords:
fine particles. It was found that the presence of particles did not suppress dynamic recrystallization dur-
Magnesium alloys
Recrystallization
ing channel die deformation. Fine particles did lead to a much reduced recrystallized fraction after hot
Dispersoids rolling, attributed to a retardation of static recrystallization kinetics. Although the presence of pinning
particles greatly slowed recrystallization kinetics on annealing, for no conditions studied was it possible
to prevent recrystallization of the as-deformed structure using particles.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction to prevent grain growth following thermomechanical processing

Control of grain size and texture during thermomechanical
processing (TMP) is key to improving the properties of wrought
magnesium alloys [1]. In many other alloy systems, particles are
used to help provide this control. For example, coarse particles
may be deliberately used to promote recrystallization and texture
change through particle stimulated nucleation of recrystallization
(PSN) [2]. The potential to use PSN for this purpose in wrought mag-
nesium alloys is discussed in a companion paper [3]. Many wrought
alloy systems also make use of fine particles, usually referred to as
dispersoids, for the purpose of grain structure control. For exam-
ple, in wrought aluminium alloys, dispersoid forming elements
are often added in commerical alloys. These precipitate early in
the thermomechanical processing sequence (e.g. during homoge-
nization heat treatment after casting) as finely distributed stable
particles that can prevent recrystallization or grain growth via the
Smith–Zener pinning effect [4].
A fine grain size is known to be particularly desirable in mag-
nesium alloys, and several studies have focussed on introducing
elements such as calcium which can form pinning precipitates
∗ Corresponding author. Tel.: +44 1613063560.
E-mail address: joseph.robson@manchester.ac.uk (J.D. Robson).
1
Present address: Magnesium Elektron UK, P.O. Box 23, Swinton, Manchester
M27 8DD, UK.
[5,6]. There have also been several studies where fine, stable,
particles have been introduced into magnesium alloys through
modifications to alloy chemistry and processing, usually for the
purpose of directly enhancing mechanical properties such as creep
resistance [7]. Manganese is a common choice of precipitate form-
ing element in magnesium where thermal stability is critical. It has
low solubility and diffuses slowly in the matrix, and can be pre-
cipitated in the form of fine particles that are stable at elevated
temperature [8]. The presence of fine, stable particles, has also been
reported to lead to grain refinement after TMP (e.g. [9,5,6]). Here,
the particles act to refine grain size by preventing grain growth
beyond a particle limited size [5]. However, to date there has not
been a detailed study of how fine precipitate particles influence
deformation and recrystallization in wrought magnesium alloys
(prior to grain growth). In particular, it is important to differentiate
between any differences that fine dispersoid particles have on static
and dynamic recrystallization (SRX and DRX), since both are impor-
tant during TMP of magnesium. The effectiveness of such particles
in suppressing recrystallization in magnesium and whether this
can be exploited to produce improved grain structures or optimize
textures after TMP are currently poorly understood.
In this study, a simple model alloy system (Mg–Mn) is used
to develop different distributions of fine dispersoid particles, and
investigate their effects on microstructure and texture evolu-
tion during hot deformation and annealing. Previous studies have
shown that the precipitates in such alloys are close to pure man-

0921-5093/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2011.02.030
4240 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247
Table 1
Composition of the two alloys used in the present study (wt%).
Alloy Mn Zn Al Fe Si Ni
M03 0.34 0.004 0.002 0.013 0.003 0.0007
M16 1.55 0.004 0.002 0.009 0.001 0.001
agnese in composition, and that they coarsen slowly at typical
processing temperatures for magnesium, suggesting this is suitable
as a potential dispersoid forming system [8,10].
2. Experimental
Two magnesium–manganese (0.34 and 1.55 wt% Mn) alloys
were provided by Magnesium Elektron Limited, UK, in the form
of sand cast plates of dimensions 200 mm × 200 mm × 25 mm. The
full chemical compositions of these two alloys are given in Table 1.
Following casting, the alloys were subject to a range of differ-
ent heat treatments designed to produce fine, stable, dispersoid
particles of varying sizes and fractions. One group of specimens
was subject to a high temperature pre-treatment at 615 ◦ C for
8 h in a furnace with a protective SF6 atmosphere, followed
by water quenching in an attempt to maximize the amount of
manganese taken into solution prior to the precipitation heat
treatment. Another group of specimens were given the precip-
itation heat treatment directly after casting without solution
heat treatment. To determine the precipitation kinetics, a range
of precipitate heat treatments were performed at temperatures
of 300, 400, and 500 ◦ C for times ranging from 5 min to 8 h.
These heat treatments were used to develop an approximate
time–temperature–transformation (TTT) diagram for manganese
particle precipitation, which was then used to select heat treat-
ments for further study.
It was found that heat treatment directly from the as-cast state
of between 3 and 7 h at 300 ◦ C gave dispersoid particle distributions
in alloy M16 with an expected maximum pinning effect, and sub-
sequent work was performed on material in this condition. These
samples are given the designation ‘N’ (non-solutionized).
The heat-treated samples were deformed by either hot rolling
or plane strain compression using a channel die rig. Channel die
specimens were compressed in an Instron 4505 compression test-
ing machine fitted with a custom made rig. The samples, which
were 10 mm × 10 mm × 12 mm in size, were coated three times in
graphite lubricant and compressed with an initial strain rate of
10−3 s−1 . Deformation was performed at 350 ◦ C to final true strains
between 0.4 and 1.2 followed by quenching into water to preserve
the microstructure in its as-deformed state. Due to restrictions of
the test rig used, up to 3 s elapsed between the end of deforma-
tion and the completion of the quench. Quenched specimens were
removed for examination and annealing was then performed at
400 ◦ C for times of up to 6 h, followed by rapid quenching.
Specimens for unidirectional rolling were prepared by skim-
ming 2.5 mm from the surface of the cast ingots and cutting to
produce blocks of 60 mm × 60 mm × 20 mm.
These specimens were rolled down to 5 mm thickness in seven
passes. The pass schedule was designed to give a constant incre-
ment in true strain for each pass, with an initial reduction in
thickness of 4.4 mm. Prior to rolling, the specimens were held in
a furnace pre-heated to 450 ◦ C for 30 min and between passes
specimens were returned to the furnace until they again reached
450 ◦ C (which took approximately 15 min). Following completion
of rolling, specimens were quenched in water. Some of the material
was then annealed at 400 ◦ C for times of up to 2 h.
The microstructures of the as-received, deformed and annealed
specimens were studied by the use of optical microscopy and scan-
ning electron microscopy (Philips XL30 FEGSEM). Second phase
particles were investigated by use of SEM and transmission electron
microscopy (Philips CM200 TEM) and were characterized using
Mg energy dispersive X-ray spectrometry (EDX). The particle size and
Bal distribution were quantified using Image J computer software [11].
Bal Information about grain orientation and texture was obtained by
use of the electron backscattered diffraction (EBSD) technique.
EBSD data were used to produce orientation maps colored by
Euler angle with high angle grain boundaries (>15◦ misorientation)
marked as thick black lines and low angle grain boundaries (>1.5◦ )
as thin black lines.
For optical microscopy, samples were mechanically ground and
polished, finishing was done with an oxide particle suspension
(OPS) polish. The samples were first etched to reveal grain bound-
aries using 2% Nital and then submerged in a picric-acid etch
containing 10 mg picric acid, 5 ml acetic acid, 10 ml water and
100 ml ethanol.
Following mechanical polishing, the samples for EBSD were
electropolished using a solution consisting of 75 ml nitric acid
(conc. 69%) and 175 ml ethanol cooled to −30 ◦ C at 12 V for 30–40 s.
EBSD data were acquired in the FEGSEM operating at 20 kV, with a
sample tilt of 70◦ and a working distance of 20 mm. A step size of
0.2 ␮m was used for the study of deformation zones and 0.5 ␮m for
the production of all other orientation maps. Backscattered diffrac-
tion patterns were collected using a charge-coupled deviced (CCD)
camera and interpreted using the Flamenco acquisition program
from hkl software.
3. Results
3.1. Particle distributions
An approximate TTT diagram for manganese particle precipi-
tation in solution treated alloy M16 was produced corresponding
to the time taken for observation of the dispersoid particles in
the FEGSEM after precipitation heat treatment. The microstruc-
ture obtained after solution treatment (Fig. 1(a)) contains some
large constituent intermetallic particles that consist of iron and
manganese, discussed in detail in the companion paper on coarse
particle effects [3]. These particles are insoluble and remove some
of the manganese available for precipitation from the matrix. They
are present in both M03 and M16 alloys. After precipitation heat
treatment, fine rod shaped particles are also observed within the
grains.
Fig. 1(b) shows a TEM image of these particles, revealing
their morphologies. However, this image corresponds to material
directly heat treated after casting without a prior solution treat-
ment for 3 h at 300 ◦ C. This direct heat treatment led to more
rapid precipitation and a higher particle volume fraction (discussed
below) than in pre-solution heat treated material, believed to be
due to a loss of solute manganese to coarse insoluble constituents
during the solution treatment. EDX measurements (reported else-
where [12]) confirm that as expected, in all conditions the fine
particles are close to pure manganese in composition.
The approximate TTT diagram for precipitation of fine man-
ganese particles from the solution heat treated material is shown in
Fig. 1(c). The minimum particle diameter for reliable observation at
the magnifications used in the FEGSEM in this study was 50 nm, and
the TTT curve therefore represents (approximately) the minimum
time to observe particles above this critical size. As mentioned,
the prior solution heat treatment led to retardation of precipita-
tion, so that for example 3 h at 300 ◦ C was insufficient to produce
detectable precipitation in the FEGSEM when a prior solution treat-
ment was used. The upper limit to the TTT curve is determined by
the solvus temperature, calculated using a Calphad model (JMat-
Pro [13]) which accounts for the manganese removed into coarse
 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247 4241

Fig. 1. (a) Optical micrograph of alloy M16 after solution treatment (etched) showing retained large insoluble particles and the initial large grain size. (b) TEM image of fine
manganese needles in alloy M16 after direct aging (no solution treatment) for 3 h at 300 ◦ C. (c) Approximate TTT diagram for observable fine manganese particle precipitation
in alloy M16 with prior solution treatment.

iron–manganese constituent particles. The nose of the TTT-curves
falls between approximately 500 and 550 ◦ C. However, at 500 ◦ C
the number density of precipitates was low compared to that at
lower temperature and the particles formed were large and widely
spaced.
The pinning effectiveness of a particle distribution in preventing
grain boundary migration is expected to depend on the volume
fraction to radius ratio according to the Zener pinning equation
[2]. It was found that heat treatment at 300 ◦ C gave a particle size
distribution that maximized this ratio whilst retaining a reasonable
precipitation time (a few hours). This temperature was therefore
used to generate particles for deformation and annealing studies.
Alloy M03 did not form any detectable fine particles at 300 ◦ C even
after 8 h (the longest precipitation time studied).
Fig. 2 shows the distribution of fine particles for alloy M16 after
precipitation treatment for 3 h at 300 ◦ C, with (a and c) and without
(b and d) prior solution treatment. The low magnification micro-
graphs (a and b) reveal extensive heterogeneous precipitation has
occurred both within the grains and along grain boundaries. The
large particles within the grains and along grain boundaries were
predominantly the iron and manganese rich intermetallic con-
stituent phases. The initial grain size of the specimens was very
large (e.g. 525 ␮m in alloy M16) since no grain refiner was used.
Fig. 2 also shows fine scale precipitation within the grains formed
during the 3 h precipitation treatment. The number density of these
precipitates is much greater in the material which did not undergo
a high temperature pre-treatment (Fig. 2(d)). However, since this
precipitation occurred directly from a segregated cast structure it
is highly heterogeneous. In particular, bands of intense precipita-
tion of rod shaped particles occur within the grains, as seen at low
magnification (b), and the fine scale precipitates exhibited in (d)
are characteristic of the microstructure between these bands.
Image analysis was used to calculate the average effective par-
ticle radius (the radius of the equal area circle for needle shaped
particles) and local volume fraction, and hence the local volume
fraction to radius (Vf /r) ratio. This analysis clearly ignores the effect
of the non-spherical particle shape on pinning effectiveness, but
since the purpose of the calculation was to provide a qualitative
ranking of the expected pinning effect rather than an accurate
determination of the pinning pressure, this approximation is suf-
ficient. Note that the measured local volume fraction of particles
often greatly exceeds the maximum average volume fraction that
the manganese particles was non-uniform, leading to large local
variations in Vf /r.
The calculated Vf /r ratios from these measurements there-
fore represent maximum values, since there are regions of the
microstructure with a lower volume fraction of precipitates, and
hence lower pinning effect. Non-uniformity of pinning due to pre-
cipitation from segregated structures is well known in aluminium
alloy dispersoid containing alloys, and has an important effect on
recrystallization resistance, since regions depleted in dispersoids
can recrystallize much more easily than those that are enriched
[14]. Although performing the initial solutionizing improves the
uniformity of the particles within the grains, this was accompa-
nied by a reduction in the volume fraction and an increase in the
particle size, leading to an overall reduction in Vf /r at all posi-
tions. This can be attributed to a loss of manganese to the insoluble
iron–manganese intermetallics that increase in fraction during high
temperature heat treatment [3].
Table 2 summarizes the Vf /r measurements for the manganese
precipitates. The largest Vf /r was measured after direct heat treat-
ment from casting for 3 h. This heat treatment was given the label
N3, and thus the alloy and heat treatment combination giving man-
ganese particles with the maximum Vf /r ratio is referred to as
M16–N3. In addition to the pinning pressure retarding boundary
migration due to particles (which depends on the Vf /r ratio), the
Zener limited grain size is also an important concept [2]. This is
the mean grain size at which the driving pressure for grain growth
will be balanced by the particle induced pinning pressure, leading
to a stagnation of the grain growth process. Although this con-
cept is difficult to apply when particle distributions are highly
heterogeneous, as in this study, it is still of interest to estimate
an approximate Zener limited grain size from the mean particle
volume fraction and radius. Classically, the Zener limited grain
diameter (DZ ) is approximated as [2]:
4r
DZ = (1)
3Vf
The calculated values for DZ are reported in Table 2.
Table 2
Local maximum volume fraction (Vf ), equivalent area mean radius (r̄), pinning effec-
tiveness (Vf /r) of particles within the grains, and Zener limited grain diameter (DZ )
for alloy M16 after different heat treatments.

is possible from equilibrium calculations based on the average alloy Heat treatment Vf (%) r̄ (nm) Vf /r DZ (␮m)
composition. This is attributed to the large effect of manganese (mm−1 )
segregation in the cast structure, with regions enriched in man- 615 ◦ C, 8 h + 300 ◦ C, 3 h 0.5 89 56 23.8
ganese able to form a higher fraction of particles than expected 615 ◦ C, 8 h + 300 ◦ C, 7 h 1.0 58 172 7.8
from a consideration of the average alloy chemistry alone. Even in 300 ◦ C, 3 h 3.6 34 1059 1.3
300 ◦ C, 7 h 4.4 43 1023 1.3
the specimens given a prior solution treatment, the distribution of
4242 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247
Fig. 2. Distribution of manganese precipitates in alloy M16 after precipitation treatment for 3 h at 300 ◦ C: (a and c) with prior solution treatment (low and high magnification
respectively); (b and d) direct aging from casting (low and high magnification respectively).
3.2. Channel die deformed material
Fig. 3 shows typical EBSD maps after deformation (in this case,
to a true strain of 0.53). The very large starting grain size prior
to deformation promotes the formation of heterogeneities in the
deformed microstructure. These include twins and extensive shear
bands. These features are discussed in more detail in the companion
paper [3] where the same alloys were used to study the influence of
coarse particles by using a different heat treatment. Similar features
were observed in the specimens used in this work, despite the very
different particle distributions.
The EBSD maps reveal that partial DRX has occurred in both
alloys, irrespective of the presence of a high number density of
manganese particles in alloy M16–N3. As typically observed for
magnesium alloys, DRX is confined to the mantle regions of the
original grains, shear bands, and twins. The highly heterogeneous
nature of recrystallization in these alloys made it difficult to make
an accurate quantitative comparison of the recrystallized frac-
tion. However, there was no systematic trend observed between
expected particle pinning (Vf /r ratio) and the fraction of DRX
observed. Indeed, as Fig. 3 shows qualitatively, M16–N3 contains
regions where the fraction of DRX is greater than that in M03,
free of fine particles. There were no other clear differences in the
microstructures of the channel die specimens deformed in the pres-
ence or absence of manganese pinning particles, despite the large
difference in average particle pinning pressure. It appears (as Fig. 3
shows) that the DRX grain size in M16–N3 was smaller than that in
M03, but since the DRX grain sizes vary widely from place to place
it was not possible to prove this quantitatively with a high level of
confidence.
Annealing studies revealed that even in M16–N3, static recrys-
tallization was not prevented, although the kinetics of static
annealing were greatly slowed. For example, after 1 h annealing,
alloy M03 was fully recrystallized, whereas alloy M16 remained
largely unrecrystallized [12]. For example, EBSD maps for alloys
M03 and M16–N3 after 1 h annealing show this effect (Fig. 4), with
a very large difference in recrystallized fraction during the early
stages.
However, longer annealing of alloy M16–N3 led to a progres-
sive further increase in recrystallized fraction. Fig. 5 shows a series
of optical micrographs at increasing annealing time revealing an
increase in the fraction of recrystallization. Quantitative analysis of
the effect of pinning particles on annealing kinetics was performed
in more detail on the rolled material, as discussed in the following
section. However, the critical observation was that although the
particle pinning effect slowed the kinetics of recrystallization, in no
cases studied was it sufficient to prevent further static recrystalliza-
tion on annealing. To determine if this was due to a loss of pinning
effectiveness due to particle dissolution and coarsening, particle
distributions were examined post-anneal. However, as expected
given the known slow diffusivity of manganese in magnesium,
the mean particles size and number were only slightly altered,
and in some cases (including the M16–N3 material) the Vf /r ratio
increased slightly during the anneal due to some additional precipi-
tation of manganese particles, suggesting that sufficient manganese
supersaturation was left in solution for some further precipitation.
 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247 4243

Fig. 3. EBSD maps of channel die deformed specimens: (a) alloy M03; (b) alloy M16. Both alloys were heat treated for 3 h at 300 ◦ C directly from casting.

Further details of the particle evolution are given elsewhere [12],
but it was clear that particle instability during annealing is not a
significant factor in determining the observed poor effectiveness
in preventing recrystallization during static annealing.
3.3. Rolled material
Fig. 6 shows optical micrographs and EBSD maps of the as-rolled
grain structure for the M03 alloy free of fine manganese particles
(a and b) and M16–N3 alloy (c and d). Unlike in the case of channel
die deformation, there are clear differences in the microstructures
obtained directly after rolling. The microstructure of alloy M03 con-
sists largely of near equiaxed grains free of twinning or intense
sub-structure, separated by remnants of the original grains, which
contain twins of a variety of characters (discussed in detail else-
where [12]). It is likely that these grains formed by DRX in the last
rolling pass, probably followed by rapid metadynamic recrystal-
lization/grain growth in the short time taken for the specimen to
exit the rolling mill and enter the quench since the recrystallized
grains have become quite large (grain diameters up to 50 ␮m).
In alloy M16–N3 the as-rolled microstructure is dominated by
heavily twinned, deformed large grains. Some fine grains can be
seen decorating the grain boundaries of the large grains, formed
by DRX in the final rolling pass. These DRX grains present are gen-
erally small (<10 ␮m diameter) although there is evidence in the
optical micrograph for infrequent, isolated occurrences of larger
DRX grains.
Fig. 7 shows EBSD maps of alloys M03 and M16–N3 after 1 h
annealing at 400 ◦ C. In both cases, extensive recrystallization has
occurred. In alloy M03, a fully recrystallized structure was obtained,
and extensive grain growth has taken place, leading to some large
grains (up to 80 ␮m in diameter). In alloy M16–N3, the unrecrys-
tallized microstructure obtained after rolling was largely replaced
by recrystallized grains, with some small unrecrystallized regions
remaining. However, the grain structure is markedly different from
that obtained in alloy M03. In particular in M16–N3 a very hetero-
geneous grain structure can be seen, with clusters of fine grained
regions separated by regions of larger grains. The size of the largest
grain, however, is less than half that in M03, suggesting a retarda-
tion of grain growth.
Fig. 8 shows the measured evolution of recrystallized fraction
with annealing time for M03 and M16–N3. As discussed, in the
as-rolled condition, there is a large reduction in the recrystallized
fraction in the fine particle containing alloy (M16–N3). However,
even in this alloy, initial static recrystallization occurs rapidly at
400 ◦ C, so that after 30 min of annealing, the recrystallized fraction
is over 60%. At longer times, the recrystallized fraction increases
more slowly in both M03 and M16–N3. After 2 h at 400 ◦ C, full

Fig. 4. EBSD maps of channel die deformed specimens annealed at 400 ◦ C for 1 h (a): alloy M03; (b) alloy M16. Both alloys were heat treated for 3 h at 300 ◦ C directly from
casting.
4244 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247
Fig. 5. Alloy M16 after (a) channel die deformation following heat treatment for 3 h at 300 ◦ C and subsequent annealing at 400 ◦ C for (b) 2 h, (c) 6 h and (d) 12 h.
recrystallization has occurred in alloy M03, and the recrystallized
fraction in M16–N3 has reached 75% but has not fully stagnated.
4. Discussion
Precipitation heat treatment of binary Mg–Mn alloys in alloy
M16 leads to the formation of fine rod shaped particles that are
close to pure manganese in composition. The most rapid precipita-
tion kinetics occur close to the solvus temperature, but to maximize
the Vf /r ratio of the particle dispersion whilst obtaining precipita-
tion in a reasonable time, a heat treatment temperature of around
300 ◦ C is optimum. Performing a high temperature solution heat
treatment prior to precipitation does not appear to be beneficial
and it is suggested that this is due to loss of manganese to coarse
constituent iron–manganese particles on the grain boundaries at
the solution treatment temperature.
With or without prior solution treatment, the manganese par-
ticles are heterogeneously distributed within the microstructure.
Precipitate free zones (PFZs) form adjacent to grain boundaries
and in the non-solutionized material, a bimodal banded precipi-
tate distribution is obtained. The preferential precipitation of coarse
manganese containing particles on the grain boundaries that draw
solute from the surrounding grains is likely to be the main factor
leading to PFZ formation. Prior to solution treatment, manganese
would also be expected to be segregated towards the dendrite
centres, since the Mg–Mn system is characterized by a peritec-
tic reaction; this phenomenon is similar to the well understood
distribution of dispersoids that form in the aluminium–zirconium
system, which is shown to be peritectic [15]. The banded struc-
tures observed on direct precipitation treatment is presumably
a result of the microsegregation of manganese in the casting,
since these banded structures were not observed if a solution heat
treatment was performed. However, this point was not studied
further.
The maximum Vf /r ratio for the manganese particles, deter-
mined for the M16–N3 condition, was 1059 mm−1 . This is greater
than the typical Vf /r ratios reported for dispersoids in alu-
minium alloys where recrystallization is completely suppressed
(e.g. 350 mm−1 in AA7050 with 0.13 wt% Zr + 0.1 wt% Sc [15]).
Such a distribution might therefore be expected to provide potent
inhibition of recrystallization. However, as-deformed specimens
from channel die studies reveal that the presence or absence
of manganese pinning particles has very little influence on the
as-deformed recrystallized fraction. This recrystallization occurs
predominantly in the grain mantle regions. These regions are
depleted in manganese particles (PFZ) and thus it is likely that
the initiation of DRX at prior grain boundaries is not inhib-
ited.
The PFZ width is typically around 1–10 ␮m, whereas the recrys-
tallized regions are up to 80 ␮m in width, even in alloy M16–N3.
It is therefore clear that the pinning provided by the parti-
cles is insufficient to prevent recrystallization outside the PFZ.
This becomes clear on annealing, where the recrystallized frac-
tion increases still further, demonstrating the particle pinning
is insufficient to overcome the stored energy driving recrystal-
lization. The present observations show that the presence of a
pinning particle distribution with a Vf /r ratio that would be con-
sidered large for a dispersoid system in aluminium alloys (and
would probably enable a fully unrecrystallized microstructure to
be maintained in such alloys [15]) is insufficient to prevent DRX
 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247 4245

Fig. 6. Alloy M03 heat treated for 3 h at 300 ◦ C after hot rolling: (a) optical micrograph and (b) EBSD map. Alloy M16 after the same heat treatment and hot rolling procedure:
(c) optical micrograph (d) EBSD map.

in magnesium or subsequent static recrystallization on anneal-
ing.
In rolled material, where the strain rate is much higher, the pres-
ence of fine manganese particles has had a marked effect on the
deformed microstructure. In the particle free alloy, the as-rolled
material was largely recrystallized but in the particle contain-
ing case a largely unrecrystallized microstructure was obtained.
In the temperature and strain rate regime used for rolling (strain
rate = 0.98 s−1 ), metadynamic recrystallization on exiting the rolls
is expected to be very rapid and can lead to a large increase in grain
size and recrystallized fraction even in the very short time (1 s) prior
to the quench [16]. The observation that annealing of the particle
containing alloy leads to extensive further recrystallization demon-
strates that the largely unrecrystallized as-rolled structure is not a
result of complete pinning of the boundaries. Rather, it seems most
probable that the influence of the particles is mainly a kinetic effect;
the inhibition they provide to boundary migration slows recrys-
tallization. This enables a largely unrecrystallized structure to be

Fig. 7. Heat treated (3 h at 300 ◦ C) and hot rolled material after annealing for 1 h at 400 ◦ C: (a) alloy M03; (b) alloy M16.
4246 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247

grain structure, which itself depends on deformation conditions

100 M0 3 and post-deformation cooling.
M1 6 Finally, in no case was it possible to generate a particle dis-
tribution that was effective in fully pinning the deformed grains
Recrystallized fraction / %

80
and preventing recrystallization on annealing. This suggests that
for the deformation conditions used in this study (both rolling
and channel die), the driving force due to the stored energy in
60
the deformed structure is always sufficient to overcome the par-
ticle pinning pressure. The Vf /r ratio obtained in the Mg–Mn alloy
M16–N3 is high for a dispersoid forming system (much larger than
40
that for effective dispersoid systems in aluminium alloys) and the
Mg–Mn system is likely to be one of the best dispersoid forming
20
systems in magnesium. Given that this is insufficient to prevent
static recrystallization, this work suggests that it may not be pos-
sible to develop particle stabilized deformed microstructures in
0 magnesium alloys after industrial deformation processes as can be
As−def. 0.5h 400C 1h 400C 2h 400C obtained in aluminium alloys.

Fig. 8. Recrystallized fraction as a function of annealing time for alloy M03 and M16
after prior heat treatment (3 h at 300 ◦ C) and hot rolling. 5. Conclusions

The effect of fine manganese particles on the dynamic and

retained after rolling in the particle containing alloy, although this static recrystallization in magnesium–manganese alloys was inves-
is unstable and sufficient stored energy remains to drive further tigated for specimens deformed at slow strain rate (channel die)
recrystallization during subsequent annealing. and higher strain rate (hot rolling). The following conclusions may
The grain sizes obtained after DRX and static annealing also be drawn from this work:
greatly exceed the calculated Zener limited grain size, which for
the maximum pinning case was calculated as 1.3 ␮m. This is again
• A 300 ◦ C precipitation heat treatment is able to generate a distri-
considered to be due largely to the highly heterogeneous distribu-
bution of fine manganese particles that are resistant to coarsening
tion of the pinning particles. There are regions of the microstructure
and dissolution during subsequent rolling and annealing for the
depleted in particles where the grains are able to grow much larger
conditions used in this study.
than that this calculation would suggest. These regions are then
• The maximum expected pinning effect (as characterized by the
able to impinge to produce a recrystallized structure, which has a
volume fraction to radius ratio of the particles) is greatest when
grain size larger than that calculated when microstructural hetero-
heat treatment is performed direct from the as-cast structure
geneity is ignored. The large variations in grain size with position,
rather than with a pre-solution treatment. A precipitate free zone
even after long annealing, are evidence that in some regions grain
is obtained adjacent to grain boundaries (with or without solution
growth is much more effectively halted by particles than in others.
treatment).
A comparison between the results from the channel die and
• The optimized precipitation heat treatment leads to a particle dis-
rolling experiments demonstrates that the observed behaviour is
trbution capable of producing a maximum pinning pressure that
strain rate sensitive. An important consideration is the different
is greater than that achieved in aluminium alloys where recrys-
influence that particles will have on DRX as opposed to meta-DRX
tallization under normal rolling conditions can be completely
or static recrystallization/grain growth. This is not well understood
suppressed.
for magnesium alloys. The slow strain rate used in the channel die
• The presence of a fine particle dispersion has little effect on the
tests allows time for extensive DRX to occur. There are various
fraction of dynamic recrystallization obtained after channel die
mechanisms proposed for DRX in magnesium [17]. At the tem-
deformation under the conditions studied.
perature and strain rate range used for channel die deformation
• The presence of a fine particle dispersion does allow a largely
in this study, bulging of prior grain boundaries is the likely first
unrecrystallized structure to be retained after hot rolling under
stage for DRX [17]. Since this bulging can occur in the PFZ adjacent
conditions where an alloy without such a dispersion is largely
to the grain boundaries, the presence of particles elsewhere in the
recrystallized. This is attributed to retardation of the recrystal-
microstructure would not be expected to prevent the initiation of
lization kinetics rather than stabilization of the unrecrystallized
DRX. In the heavily deformed grain mantle regions, the observa-
structure.
tions suggest that the particles are unable to prevent these DRX
• Annealing after channel die deformation or hot rolling leads
grains from growing beyond the PFZ, and new DRX grains forming.
to extensive further recrystallization even when a fine parti-
Indeed, the presence or absence of particles has little effect on the
cle dispersion is present. The kinetics of this recrystallization
DRX fraction when the time available for DRX is long (due to a slow
are dependent on the particle dispersion, being much slower
strain rate).
when pinning particles are present. However, in no case studied
During rolling, the time for DRX is much less, but the kinet-
were fine particles able to prevent static recrystallization during
ics for meta-DRX/static recrystallization after rolling are expected
annealing after deformation.
to be much faster [16]. The time available for these processes to
operate, post-deformation but pre-quench is very short (1 s in
this study). By slowing boundary migration, the particles are able Acknowledgements
to suppress these static processes sufficiently so that a largely
unrecrystallized grain structure is preserved. It is thus suggested This work was funded by the EPSRC Portfolio Partner-
that particles are more effective in suppressing static recrystalliza- ship on Light Alloys for Environmentally Sustainable Transport
tion processes in magnesium than DRX. Thus their influence on (EP/D029201/1) and Magnesium Elektron. Magnesium Elektron is
the final microstructure will depend on the relative importance of thanked for the provision of materials used in this study. Tim Wilks,
DRX and meta-DRX/static recrystallization in determining the final Paul Lyon and Gordon Lorimer are thanked for valuable discussions.
 J.D. Robson et al. / Materials Science and Engineering A 528 (2011) 4239–4247
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