Journal of Alloys and Compounds 642 (2015) 185191

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Journal of Alloys and Compounds

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

Investigation of the dependence of deformation mechanisms on solute

content in polycrystalline MgAl magnesium alloys by neutron
diffraction and acoustic emission
K. Mthis a, J. Capek a,, B. Clausen b, T. Krajnk a, D. Nagarajan c
a
b
c

Department of Physics of Materials, Faculty of Mathematics and Physics, Charles University, Ke Karlovu 5, 121 16 Prague, Czech Republic
Los Alamos National Laboratory, Lujan Neutron Scattering Center, Los Alamos, NM 87545, USA
Advanced Forming Research Centre, University of Strathclyde, 85 Inchinnan Drive, Renfrew PA4 9LJ, Glasgow, United Kingdom

a r t i c l e

i n f o

Article history:
Received 22 December 2014
Received in revised form 17 February 2015
Accepted 23 March 2015
Available online 20 April 2015
Keywords:
Magnesium
Neutron diffraction
Solution hardening
Twinning
Non-basal slip

a b s t r a c t
Inuence of aluminium content on the deformation mechanisms in MgAl binary alloys has been studied
using in-situ neutron diffraction and acoustic emission technique. It is shown that the addition of the
solute increases the critical resolved shear stress for twinning. Further, the role of aluminium on the solid
solution hardening of the basal plane and softening of non-basal planes are discussed using results of the
convolutional multiple peak prole analysis of diffraction patterns. The results indicate that the density
of both prismatic hai and pyramidal hc + ai dislocations increases with increasing alloying content.
2015 Elsevier B.V. All rights reserved.

1. Introduction
The application of magnesium alloys as lightweight structural
elements in the transportation industry has been signicantly
increased in the last two decades. However, there are many technological challenges, as e.g. limited room temperature formability
or asymmetric response on the strain path changing, which still
waiting on the proper solution. The specic deformation behavior
of the hexagonal closed packed (hcp) structure of magnesium is
often in the background of these problems. It is well known that
 0i (BE) and f1 0 1
 2g extension twinning
the basal slip 0 0 0 1h1 1 2
requires the lowest activation stress at room temperature. The
 0gh1 1 2
 0i prismatic
further slip systems, as rst-order f1 0 1


(PrE), followed by the rst- f1 0 1 1gh1 1 2 0i (PyE) and second 2gh1
1
 2 3i) pyramidal generally requires either higher
order (f1 1 2
applied stress and/or elevated temperatures to be activated. As it
was shown by numerous authors, the addition of solute elements
signicantly inuences the deformation mechanisms both in single- [1,2] and polycrystals [37]. There is a general agreement that
addition of Al and Zn increases the critical resolved shear stress
(CRSS) for basal slip and concurrently decreases that for prismatic
slip. The concentration dependence of CRSS usually follows the
Corresponding author. Tel.: +420 221 911 619; fax: +420 221 911 490.
E-mail address: jan.capek@centrum.cz (J. Capek).
http://dx.doi.org/10.1016/j.jallcom.2015.03.258
0925-8388/ 2015 Elsevier B.V. All rights reserved.

Dss / cn equation, where c is the atom concentration and n = 1/

22/3 (for dilute and concentrated alloys, respectively). The works
dealing with the inuence of solute content on the twinning mechanisms are less frequent [3,4,6,7]. The majority of above listed
works evaluates the CRSS of particular slip systems from the
stressstrain curves and the input parameters of theoretical calculations are usually also based on the single crystal data [8,9].
Nevertheless, in the case of concentrated polycrystalline alloys
such an approach often leads to ambiguous results, since the
microstructural parameters, as grain size or initial texture have
to be taken into account. In the last decade, the in-situ neutron
diffraction (ND) has been proved as proper method for investigation of deformation mechanisms in the magnesium alloys [10
12]. The large penetration depth of the thermal neutrons facilitates
the investigation of relatively large sample volumes, which is a key
feature in the case of coarse-grain materials. In combination with
the acoustic emission (AE) technique, the twin nucleation (AE measurement) and growth (ND measurement) can be successfully
investigated [10,12]. Further, the activation stresses of particular
deformation mechanisms can be deduced from the stress dependence of lattice strains. Finally, the recent results show that the
evolution of the dislocation structure can be obtained using the
diffraction line prole analysis [1315].
In this work the effect of Al on the deformation mechanisms in
binary MgAl alloys has been studied in-situ using neutron

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K. Mthis et al. / Journal of Alloys and Compounds 642 (2015) 185191

diffraction and acoustic emission techniques during uniaxial compression tests at room temperature. The inuence of the solute
content on both dislocation slip in particular systems and extension twinning is discussed in detail.
2. Experimental procedure and processing methods
Pure Mg, binary Mg2 wt.% Al and Mg9 wt.% Al (further referred as Mg2Al and
Mg9Al) were used for the experiments. Since the grain size signicantly inuences
the twinning activity, the authors endeavored to prepare specimens with similar
grain sizes. The nal (after heat treatment) grain sizes (measured by linear intercept
method according to ASTM E112) of (100 10) lm for pure Mg and Mg9Al and
(85 15) lm for Mg2Al were achieved as follows: in the casting phase 1 wt.% Zr
was added to the melt in the case of pure Mg, whereas different cooling rates were
used in the case of MgAl binary alloys. The as-cast specimens were then solution
heat treated for 24 h@413 C and quenched into water. Since the proper tuning of
cooling rate was difcult, there is a difference between the grain sizes of Mg2Al
and Mg9Al alloys. Nevertheless, such a difference is not signicant from the point
of view of the deformation mechanisms studied. The inverse pole gures (IPF)
and the microstructures after the heat treatment are showed in Figs. 1 and 2. As
it is obvious from IPFs (Fig. 1), all of specimens exhibited a random initial texture.
The initial microstructure is similar for pure Mg and Mg9Al samples (Fig. 2a and c):
the grain size varies; both coarser and ner grains are present. In contrast, the
Mg2Al specimen has more uniform grain size distribution and generally ner grains
(Fig. 2b). The testing was carried out using cylindrical specimens with a diameter of
9 mm and gauge length of 20 mm. The in-situ neutron diffraction (ND) measurements were carried out at the SMARTS engineering instrument [16] in the Lujan
Neutron Scattering Center. The mutual orientation of the longitudinal axis of the
sample and the incident beam was 45. The two detector banks were positioned
at 90 to the incident beam in order to record diffraction pattern in both along
and perpendicular to the loading direction (for scheme of the experimental setup
see [17]). The compression testing were carried out using a horizontal 250 kN
capacity load frame at a strain rate of 1  103 s1 in strain control mode. In order
to collect ND data with good enough statistics, the test were stopped at predened
strain levels (0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%) for approx. 70 min.
The acoustic emission (AE) testing was performed using a Physical Acoustics
PCI-2 acquisition board and a broadband AE sensor from Dakel company was
mounted on the outside the gauge length using vacuum grease and an elastic band.
The AE amplied by 60 dB in the frequency range 1001200 kHz. The threshold
level was set as 30 dB. The AE was recorded separately during uniaxial deformation
at the same condition, as during ND testing.
The samples for metallography were rst grinded, than polished step-by-step 3,
1 and 1=4 lm diamond paste and nally etched in 3% Nital solution.
Fig. 1. The IPF of initial texture of deformed samples measured by ND in axial
direction for (a) Mg; (b) Mg2 wt.% Al; and (c) Mg9 wt.% Al alloy.

3. Results and discussion

3.1. Stressstrain curves and the corresponding AE responses
The inuence of Al content on the mechanical properties is presented in Fig. 3. In agreement with the literature data [1,5], the
strength of alloys increased with the increasing Al content. As it
was discussed in detail by Cceres and Rovera [5], the effect of
solid solution on the yield strength in polycrystals can be roughly
deduced similarly to the single crystals, when the experimental
yield stress data are corrected for the grain size. They suppose to
express the combined effect of the grain size and solid solution
strengthening on the experimentally established yield stress rexp
02
as:
1=2
rexp
MBn cn
02 DrHP Drss r0 kd

where r0 and k are parameters of HallPetch equation (we used values r0 = 11 MPa [18], k = 0.39 MPa/m1/2 [19]), M is the Taylor orientation factor and Bn = dsR/dcn is the solid solution hardening rate
on the basal plane. In Fig. 4, both the concentration dependence of
rexp
02 as well as the values corrected to grain size Drss are plotted as a
function of the c2/3 (i.e. we assuming Labuschs theory for concentrated alloys, describing dependence of resolved shear stress Dss
on solute concentration c as Dss / c2/3 with Bn = 39.5 MPa (at.)2/3
[5]). The dependence is clearly linear and the value for M = 4.7
obtained from the linear t (slope = 185.6 MPa (at.)2/3, thus
M = 185.6/39.5) is in the range (46) suggested by theoretical calculations [18]. Thus, it seems that the strengthening of the basal

planes by solutes signicantly contributes to the yield strength.

This conclusion is in agreement with results on other binary systems (e.g. MgZn [4,20]). Nevertheless, both single crystals studies
[2] and the recent modeling data [8,9] indicates that the prismatic
hai-slip plays also a signicant role in the plasticity around the
macroscopic yield. This mechanism is enhanced by pile-up of basal
dislocations at the end of easy glide stage, since the cross-slip
through prismatic plane becomes easier due to the stress concentration from pile-ups [21]. Hence, the investigation of the inuence
of the solutes on this system is also crucial. The AE count rates (i.e.
number of crossing of threshold level per second) corresponding to
the stressstrain curves are depicted in Fig. 5a. It is obvious that the
Mg9Al specimen has the lowest AE response, whereas the pure Mg
and Mg2Al behave similarly. The characteristic peak in the vicinity
of the yield point can be attributed to synergic effect of twin nucleation and massive dislocation motion [22,23]. Discriminating of the
twinning and dislocation density is a complex task requiring statistical analysis of the AE parameters, which is beyond of the scope of
this paper. The recent results of Vinogradov et al. [24] proved that
the straining starts with a slip of dislocation in basal plane and
the twinning is the major contributor to the above mentioned peak
of count rate. Above the yield point the count rate rapidly decreases.
This effect is caused by several issues: (i) the dislocation density
increases with increasing stress, which causes reduction of the
mean free path of dislocations. Since this parameter is proportional
to the released AE energy [25], the count rate decreases. (ii) The

K. Mthis et al. / Journal of Alloys and Compounds 642 (2015) 185191

187

Fig. 3. The true stresstrue strain curves as measured in compression for various Al
concentration.

Fig. 4. Experimental yield strength rexp

02 (solid symbols); values corrected to grain
f10:2g
size Drss (empty symbols) and inection stress ri
for {10.2} lattice strain from
the ideal elastic response as a function of c2/3 (c Al concentration).

function of the applied stress and determination of fraction of

dislocations in particular slip systems.

Fig. 2. The initial microstructure of samples for (a) Mg; (b) Mg2 wt.% Al; and (c)
Mg9 wt.% Al alloy.

twin nucleation is followed by rapid twin growth in compression

[10]. The twin growth was found inaudible for AE owing to their
slow speed [26]. It is noteworthy that the decrease of count rate
is more rapid with increasing solute content, most probably due
to faster accommodation of dislocations. If the count rate is plotted
against the true stress (Fig. 5b), it can be seen that the peak values
of the count rate are shifted toward higher stresses with increasing
Al content, which is a clear sign that the twin nucleation stress
depends on the alloy content.
In summary the mechanical tests and the AE indicate that the
solute atoms harden the basal plane, signicantly increase the dislocation density and inuence the twin nucleation stress. In the
next chapter these assumptions are veried using the neutron
diffraction technique.
3.2. Neutron diffraction measurements
The neutron diffraction experiments have been used for estimation of the twinned volume, calculation of the lattice strain as

3.2.1. Solute content dependence of twinned volume

As it was shown by seminal work of Gharghouri et al. [11], the
{10.2} extension twinning causes signicant texture changes,
which manifests with intensity changes of diffraction peaks.
Since in compression the grains having their c-axis perpendicular
to the loading axis are optimally oriented for extension twinning
the {10.0}(00.2) and {11.0}{10.3} parent (i.e. grains undergoing
twinning) daughter (i.e. twinned fraction of the parents) are
those, which characterize the most the twinning activity in the
axial detector. Thus if the extension twinning is active, the {10.0}
and {11.0} peaks decreases and the (00.2) and {10.3} increases.
Such a behavior can be seen in Fig. 6, where the relative intensity
changes determined by single peak ts with respect to the initial
(stress-free) state of the parentdaughter orientations presented.
The evaluation of the twin volume fraction can be performed by
a 2-bank Rietveld renement assuming an axisymmetric texture
[17,27,28].1 Fig. 7 shows the development of the axial distribution
function for the 00.2 peak during deformation. It is obvious that
the 00.2 intensity is almost random at the start, and strongly
increases at the center during compression, consistent with the
expected texture change due to extension twinning. From the
1
Since the initial texture is random and the uniaxial deformation is an axisymmetric operation, the radial symmetry is warranted. The renements were done using
the GSAS [26] and SMARTSware [27] software packages developed at Los Alamos
National Laboratory.

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K. Mthis et al. / Journal of Alloys and Compounds 642 (2015) 185191

changes in the area under the curve below the cross-over point we
can directly determine the twin volume fraction (TVF). Fig. 8 shows
the twin volume fraction as a function of the composition, applied
strain (a) and stress (b). It is obvious that the strain dependence of
the TVF for pure Mg and Mg2% Al is the same within the experimental error (Fig. 8a), which ts well with the AE data. In contrast,
the TVF for Mg9% Al is smaller, which indicates that there is
another signicant strain accommodation mechanism besides the
twinning. Similar dependence of twinned volume on Al content
was observed in the same set of specimens by Nagarajan et al. [7]
using analysis of metallographic pictures.
If we plot the same quantity against the applied stress, we nd
that the stress, at which the twin volume starts to grow, increases
with increasing Al content. This result can be used for an estimation of the solute strengthening of the twin growth. If we subtract,
similarly to Eq. (1), the contribution of the grain size from the
experimentally measured data, we obtain a dependence of critical
stress for twin growth on the Al content. The inuence of the solute
content on the twin growth was recently studied by Ghazisaeidi
et al. [6]. They calculated the solute twin dislocation interaction
energy by density functional theory (DFT) and predicted the solute
strengthening of the twin growth for MgAl binary system. As it is
obvious from Fig. 9, our experimental data are in good agreement
with their theoretical predictions.

Fig. 5. The AE count rates measured during compression tests as a function of (a)
strain; and (b) stress for all solute concentrations.

3.2.2. Lattice strain evolution

The elastic lattice strains were calculated using the Braggs law,
which gives relation between the scattering angle (h) and lattice
spacing (d) as follows:

2d sin h nk

The relative strain (e) is than given by differentiating of Braggs

equation:

d  d0
 cot hh  h0
d0

In the present work, we considered d0 and h0 as the lattice spacing and the Bragg angle of the corresponding lattice planes in the
stress-free material. The activation of specic deformation mechanisms emerges on the lattice strain applied stress curves as a
deviation from the straight line of Hookes elasticity. In Fig. 10
the stress evolution of the (00.2){10.0} lattice strains, related to
extension twinning, are shown with respect to the both axial and
radial detector. When the twinning become active, the soft-oriented grains (e.g. {10.0} in axial and (00.2) in radial detector,
respectively) starts to behave plastically and their curve deviate
above the ideal straight line. At the same time the conjugated
curves of hard-grains fall under this line, since they have to
accommodate larger portion of the elastic loading [29]. The ideal

Fig. 6. Relative changes of normalized integrated intensity for {10.0}(00.2) and

{11.0}{10.3} intensity pairs.

Fig. 7. Axial distribution function variation for the 00.2 pole during for Mg2 wt.%
Al alloy measured at different strains.

K. Mthis et al. / Journal of Alloys and Compounds 642 (2015) 185191

Fig. 8. Evolution of twin volume fraction for all examined Al concentrations as a

function of (a) strain; and (b) stress.

189

Fig. 10. Stress evolution of the (00.2){10.0} lattice strains as it was measured in (a)
axial; and (b) radial detector. The ideal elastic response is indicated with a dash line.

elastic behavior is violated approximately at the same stress level,

at which the both twin volume starts to grow and a maximum of
the AE response is observed (c.f. Fig. 5b).
The grains having their {10.2} planes in Bragg position with
respect to the axial detector are almost ideally oriented for basal
slip in compression (their Schmid-factor for basal slip is:
mbasal
10:2 0:43). Thus, the inection point of the lattice strain gives
estimation for the activation stress for basal hai-slip. As it is shown
in Fig. 11a, this value varies with the solute content. If we plot the
data into against the c2/3 (see Fig. 4), we got a linear dependence,
giving a slope of 168.3 MPa (at.)2/3, and M = 168.3/39.5 = 4.26,
which is almost the same value obtained from the stressstrain
curves. In the case of the {10.1} grains, the activation of the
prismatic hai-slip cannot be excluded besides the basal slip

Fig. 9. Comparison of the concentration dependence of the critical stress for twin
growth as measured experimentally (symbols) and calculated using theoretically
(theoretical data are replotted from [6]). The CRSS for basal slip is indicated as well.

Fig. 11. Stress evolution of (a) {10.2}; and (b) {10.1} lattice strains as it is measured
in axial detector. The ideal elastic response is indicated with a dash line.

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K. Mthis et al. / Journal of Alloys and Compounds 642 (2015) 185191

Fig. 12. Evolution of dislocation density with applied strain for all alloy
compositions.

prism
(mbasal
10:1 = 0.36; m10:1 = 0.34). The stresses at inection points are
higher that those for {10.2} grains, but the solute dependence exhibit a similar character (Fig. 11b).

3.2.3. Fraction of dislocations in particular slip systems

The neutron diffraction patterns obtained for the Mg samples
deformed up to the strain of 6% were evaluated by the
Convolutional Multiple Whole Prole (CMWP) tting method
[30,31]. Each diffraction pattern is tted by the sum of a background spline, the convolution of the instrumental pattern and
the theoretical line proles related to crystallite size and dislocations. Finally, the dislocation density (q), and the parameters qm
1
and qm
2 are obtained. For magnesium eleven families of slip systems
on basal (4), prismatic (2) and pyramidal (5) planes with three different Burgers vectors are considered, which are divided into three
 1 1 0i (hai type),
groups based on their Burgers vectors: b1 1=3 h2

b2 = h0 0 0 1i (hci type) and b3 1=3 h2 1 1 3i (hc + ai type) Ref. [14]
in order to reduce the number of variables. The determination of
the fractions of dislocations in the different slip system families
(fa, fc and fc+a) is performed by a computer program, which takes
advantages of the fact that the values of particular fractions have
to be positive and their sum must be equal to 1 [32]. Further details
about the CMWP tting procedure can be read in Refs. [14,31,32].
The dislocation density as a function of strain is shown in
Fig. 12. The dislocation density increases with increasing Al content. This result indicates that at higher solute concentration the
accommodation of strain by dislocations becomes more signicant.
The evaluation of the fractions of the dislocations in the particular
slip systems approved this assumption. The strain dependence of
the basal hai vs. non-basal hai-dislocations ratio is clearly inuenced by the solutes (Fig. 13a).2 If we plot the relative change of
BE/(PrE + PyE) ratio against the initial dislocation conguration
(Fig. 13b), we can see that the Mg9Al specimen increases the fraction
of the non-basal hai at the expense of basal hai dislocations. Further
the stress necessary for increasing the non-basal hai fraction is less
for alloys than that for pure magnesium (Fig. 13c). The necessity of
activation of prismatic hai slip for the macroscopic plasticity is a well
know phenomenon, described in numerous theoretical [8,33] and
experimental work [1,4,5]. The solute atoms have been found to
soften the prismatic slip system through ease the both cross slip of
dislocations and ability of dislocations to form a jog-pair [2,33].
Our results indicate that the solute softening of prismatic slip system
increases with increasing Al concentration, which is good agreement
2
Owing to the similar average contrast factors of prismatic and pyramidal hai
dislocations is difcult to make difference between them, therefore they are treated
together.

Fig. 13. (a) Strain dependence of the Basal edge (BE) Prismatic + Pyramidal Edge
(PrE + PyE) dislocations ratio; (b) Evolution of the relative change of BE/(PrE + PyE)
ratio with the strain; and (c) evolution of the relative change of BE/(PrE + PyE) ratio
with the stress.

with the ndings Akhtar and Teghtsoonian [2] in dilute MgAl single
crystals.
The inuence of the solutes on the pyramidal hc + ai-slip have
 2gh1 1 2
 3i slip
been studied only in few works [34,35]. The f1 1 2
mode is the only mechanism besides the extension twinning,
which provides elongation in crystallographic c direction. Despite
of the high critical resolved shear stress for its activation at room
temperature, several works found indication for its activity
[8,12]. The strain evolution of the ratio of hai/hc + ai dislocation is
plotted in Fig. 14. There is a jump at 1% strain for Mg2Al and
Mg9Al alloy, caused by massive activation of non-basal hai slip in
the vicinity of the macroscopic yield point. For Mg9Al alloys at
higher strain level the fraction of hc + ai dislocations signicantly
increases, whereas for Mg2Al and pure Mg the increment is very

K. Mthis et al. / Journal of Alloys and Compounds 642 (2015) 185191

Fig. 14. Evolution of the ratio of hai and hc + ai dislocations as a function of the
applied strain and Al concentration.

small. Such a large difference can be given by restricted twin

growth in Mg9Al, shown in Section 3.2.1. Since the strain cannot
be accommodated by twinning, an alternative mechanism is
required for continuing the plastic deformation, which is realized
in the form of hc + ai-slip.
4. Conclusions
The inuence of solute content on the deformation mechanisms
was investigated in MgAl binary alloys using advanced in-situ
methods. The following conclusion can be drawn:
 The stress necessary for both twin nucleation and growth
increases with increasing Al content.
 The softening effect of Al on the prismatic plane was proven.
The macroscopic yielding is accompanied by onset of prismatic
hai slip, which magnitude increases with increasing Al content.
 As a consequence of limited twin growth, the pyramidal hc + ai
slip plays a key role in the plasticity of Mg9 wt.% Al alloy.

Acknowledgements
The authors are grateful for the nancial support of the Czech
Science Foundation under the project no. GB14-36566G. JC
acknowledges the support from the Grant Agency of Charles
University, Faculty of Mathematics and Physics. This work has beneted from the use of the Lujan Neutron Scattering Center at
LANSCE, funded by the US Department of Energys Ofce of Basic
Energy Sciences. Los Alamos National Laboratory is operated by
Los Alamos National Security LLC under US DOE Contract DEAC52-06NA25396. KM is grateful to Pavel Lukc (Charles
University, Prague) and Carlos Cceres (The University of
Queensland, Brisbane) for fruitful discussions.
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