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Scripta Materialia 63 (2010) 725730

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Eect of rare earth additions on microstructure and texture

development of magnesium alloy sheets
K. Hantzsche,a J. Bohlen,a,* J. Wendt,b K.U. Kainer,a,b S.B. Yia and D. Letziga
a
GKSS Research Centre, Magnesium Innovation Centre MagIC, Max-Planck-Strasse 1, D-21502 Geesthacht, Germany
b
Hamburg University of Technology, Institute of Materials Science and Technology, Eiendorfer Strasse 42,
D-21073 Hamburg, Germany
Received 13 November 2009; revised 16 December 2009; accepted 18 December 2009
Available online 23 December 2009

AbstractRare earth elements or yttrium can weaken the strong basal textures of magnesium sheets and are of interest for the
improvement of sheet formability. The weakening of magnesium sheet textures with increasing content of Ce, Nd and Y is connected
to the solid solubility of the respective element. A relationship is drawn between the weak textures and the appearance of deforma-
tion bands with compression and double twins during rolling and a grain growth restriction during annealing of the sheets.
2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Magnesium; Rare earth; Texture; Recrystallization; Twinning

1. Introduction more dilute concentrations of RE elements together with

The use of magnesium sheets, increasingly favored
due to the weight-saving possibilities, in technical appli-
cations requires improved formability at lower tempera-
tures and reduced anisotropy of mechanical properties
compared to conventionally available sheets, e.g. from
alloy AZ31 [1]. It is recognized that the hexagonal
close-packed (hcp) lattice structure of magnesium limits
the number of active deformation mechanisms, with ba-
sal slip and tensile twinning playing an important role in
the plasticity of magnesium alloys. Strong crystallo-
graphic textures evolve during rolling such that the
majority of grains are oriented with their basal planes
in the sheet plane. Recrystallization and grain growth ef-
fects do not signicantly change the texture of these
sheets (e.g. [2]). These strong textures are responsible
for an intrinsic plastic anisotropy, low elongation and
limited formability. Materials with weaker and more
random textures, however, promise improved formabil-
ity [3].
Ball and Prangnell [4] were apparently the rst
authors who observed a weaker and more random tex-
ture after extrusion of alloy WE54. This alloy is charac-
terized by a high content of rare earth (RE) elements
including yttrium. Even magnesium sheet alloys with
* Corresponding author. E-mail: jan.bohlen@gkss.de
zinc, such as ZE10, ZEK100, ZW41, exhibit weaker tex-
tures, and the orientation spread of the basal planes is
broader towards the sheets transverse direction (TD)
rather than towards the rolling direction (RD) [57].
Generally, the weakening of the textures is attributed
to the recrystallization of those alloys which are aected
by the presence of RE elements. Although the principal
eect of the RE elements on the texture development
during recrystallization is well established, the mecha-
nisms responsible for these changes in texture are cur-
rently still under discussion.
For alloy WE54, Ball and Prangnell [4] suggested
particle-stimulated nucleation (PSN) of recrystallization
as the main mechanism weakening the texture where the
high content of alloying elements corresponds to the
appearance of a broad distribution of particles. Mac-
kenzie et al. [8] conrmed that PSN is an active mecha-
nism that contributes to the development of a weaker
texture during extrusion of WE43. However, this mech-
anism does not appear to dominate the nal texture.
Alloys with a more dilute content of RE or Y exhibit
shear bands as a result of plastic deformation as shown
by Senn and Agnew [9,10]. Within shear bands, grain
nuclei growing into the band exhibit a more random tex-
ture compared to the surrounding unrecrystallized area.
Mackenzie and Pekguleryuz [7] found a non-basal tex-
ture component along TD in the shear bands that
evolved during rolling which becomes dominant in the

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doi:10.1016/j.scriptamat.2009.12.033
726 K. Hantzsche et al. / Scripta Materialia 63 (2010) 725730
fully recrystallized microstructure. A very similar eect
was shown by Stanford and Barnett [11], who used bin-
ary MgLa and MgGd extrusions in which shear bands
contributed to a randomization of the texture or to for-
mation of a new texture component, respectively. On the
other hand, typical magnesium sheet alloys (e.g. AZ31)
also exhibit shear banding during rolling without signif-
icant texture change or texture weakening during recrys-
tallization [12].
Mackenzie et al. [8] showed that the RE elements in
WE43 change the orientation relationship for high
boundary mobility, leading to a non-basal texture. This
is consistent with a selected growth of preferred orienta-
tions causing signicant changes in the nal texture.
Such eects have been associated with solute drag or
particle pinning [1,10,13,14]. None of these eects have
been clearly veried. Stanford and Barnett [11] did not
nd signicant dierences in the texture development
of magnesium extrusions whether they added La as a
largely insoluble element or Gd as a soluble element in
magnesium. It is generally known from other metals
that even very small amounts of additional elements
can have a remarkable eect on the texture development
during recrystallization [15].
The investigation of single RE elementsCe, Nd,
Yin magnesium allows the eect of each element on
the texture development during rolling to be separately
identied. These elements exhibit quite dierent solid sol-
ubilities in magnesium, with Ce having the lowest and Y
the highest. Dierent concentrations of the respective
elements provide alloys with the RE element in solid
solution as well as alloys that form precipitates. This al-
lows the eects of the elements on the sheet microstruc-
ture and texture development during deformation as
well as during recrystallization to be investigated.
2. Experimental
High-purity magnesium, pure RE elements and Y
were used in various compositions (see Table 1) and
gravity cast into billets. Slabs 20 mm thick, 280 mm
wide 50 mm long were cut for rolling experiments. A
homogenization heat treatment of 15 h at 350 C was
carried out for pure Mg and the MgY alloys and at
550 C for the MgCe and MgNd alloys prior to roll-
ing. The rolling experiments were performed using a
rolling stand with a maximum load of 50 tons and a roll
diameter of 400 mm. Experiments were carried out at
400 C and a rolling rate of 16 m min 1. The rolling pro-
cedure consisted of 14 passes with an increasing degree
of deformation /. The degree of deformation for the
rst four passes was 0.1 followed by seven passes with
/ = 0.2. A nal gauge of 1.1 mm was reached after three
further passes with / = 0.3. After each pass, the sheets
were reheated for 20 min to keep the rolling temperature
at 400 C. After the rolling experiments the sheets were
cooled down in air. Samples of the nal sheets also re-
ceived a heat treatment for 20 min at the same
temperature.
Optical microscopy was used to analyse the micro-
structure of the sheets. Standard metallographic sample
preparation techniques were applied using an etchant
Table 1. Alloy nomenclature and composition of the cast billets.
Alloy nomenclature Ce [at.%] Nd [at.%] Y [at.%]
MgCe0.006 0.0056
MgCe0.01 0.013
MgCe0.03 0.03
MgCe0.2 0.18
MgCe0.5 0.53
MgNd0.006 0.0056
MgNd0.01 0.0102
MgNd0.04 0.041
MgNd0.08 0.08
MgNd0.2 0.17
MgNd0.3 0.34
MgY0.003 0.003
MgY0.03 0.027
MgY0.2 0.17
MgY0.3 0.28
MgY0.8 0.84
based on picric acid [16], which reveals grains, grain
boundaries and twins.
Texture measurements were performed on the sheet
mid-planes. A Panalytical X-ray diractometer setup
using Cu Ka radiation was employed to measure pole g-
ures to a sample tilt of 70. The (0 0 0 2), {1010}, {10
11}, {1120} and {1013} pole gures were measured
and used to calculate the complete orientation distribu-
tion, which allows the recalculation and presentation of
complete pole gures. Local orientation patterns were
measured by electron backscatter diraction (EBSD)
on a eld emission gun scanning microscope (Zeiss, Ultra
55, EDAX/TSL EBSD system with Hikari detector).
Samples were taken from longitudinal sections of the
sheets and prepared by mechanical polishing using alu-
mina powder, followed by electrochemical polishing.
3. Results
Figure 1a and b shows the microstructures of two
sheets, MgNd0.01 and MgNd0.2, as representative re-
sults for the as-rolled condition. A deformed microstruc-
ture with twins and grains that are partly elongated
along the rolling direction is visible as result of the com-
plex rolling procedure, especially of the nal rolling
pass. In the sheet with the low concentration of Nd,
grains appear to be larger compared to the higher-al-
loyed sheet, and areas of small recrystallized grains are
found next to large deformed grains.
After the additional heat treatment, completely
recrystallized microstructures are formed as shown in
Figure 1c and d. Again, there is a signicant dierence
in the grain size of the two sheets as a function of the
Nd content. In general, the grain size of the recrystal-
lized sheets depends on the alloying content of the
respective elements Nd, Ce and Y. Figure 2 shows the
average grain size of the heat-treated sheets vs. the alloy-
ing content. In all three series of alloys a signicant de-
crease in the average grain size is found with increasing
alloying content. A content of each element as low as
0.05 at.% leads to a maximum reduction of the grain
size, which then does not distinctively change with high-
er element content. It is notable that the average grain
 K. Hantzsche et al. / Scripta Materialia 63 (2010) 725730
Figure 1. Microstructures in as-rolled condition: (a) MgNd0.01; (b) MgNd0.08; and after annealing for 20 min at 400 C: (c) MgNd0.01; (d)
MgNd0.08.
Figure 2. Average grain size of all sheets after annealing vs. the
element content.
size of 33 lm of a pure Mg sheet is not the largest com-
pared to alloys with a very low content of additional
alloying element. However, it is still larger compared
to the grain sizes in alloys with higher alloying element
content.
In Figure 3a the recalculated (0 0 0 2)-basal pole g-
ures represent the texture of the rolled sheets for dier-
ent element contents. For all three series of alloys an
example with relatively low and relatively high element
content is selected. In all cases, a typical basal texture
evolved during the rolling experiments, which orients
the majority of grains parallel to the sheet plane or, at
higher element content, tilted towards the RD. The lat-
ter textures are typically found for magnesium sheets in
a deformed rather than in a recrystallized condition [17].
Moreover, the textures become signicantly weaker with
higher element content for all three series of alloys.
Figure 3b shows the maximum intensity taken from
the (0 0 0 2)-pole gures as a function of the element
content for the three alloy series in the as-rolled condi-
tion. Since the textures obviously do not change qualita-
tively, this intensity is taken as a measure of the
727
signicance of the texture. For all three alloy series, as
well as for pure magnesium, there is a high intensity at
low concentrations of 15 m.r.d. (multiples of random
distribution). At high concentrations a signicantly low-
er intensity of 6 m.r.d. is found for all the alloy series.
The concentration at which the intensity starts to de-
crease diers from element to element and is found to
be lowest for Ce (0.01 at.%), higher for Nd (0.04
at.%) and highest for Y (0.17 at.%). It is worthwhile
repeating that this tendency also reects the dierent so-
lid solubilities of the respective elements in magnesium:
at the rolling temperature of 400 C applied in this
study, the solubility is lowest for Ce (0.014 at.%), higher
for Nd (0.12 at.%) and highest for Y (1.87 at.%) [18].
Figure 3c shows that the drop in intensity with increas-
ing element content is not aected by the additional heat
treatment. However, there is an increase in the intensity
at low concentrations of elements and in pure magne-
sium. Furthermore, there is a decrease of the intensity
at higher concentrations.
Figure 4a and b shows EBSD orientation maps from
longitudinal sections of the as-rolled sheets from
MgNd0.01 with low element content and a strong basal
texture, and from MgNd0.04 with higher element con-
tent and a weak texture. The selected areas cover regions
with high local misorientations that are characteristic of
the microstructures. Dierent types of twin boundaries
are highlighted in dierent colours. In the MgNd0.01
sheet small recrystallized grains are observed sur-
rounded by large deformed grains that contain a small
number of dierent twins. {1012}-tensile twins are
more frequently found than, for example, {1011}- or
{1013}-compression twins or {1011}/{1012}- or
{1013}/{1012}-double twins. In contrast, the de-
formed region in the MgNd0.04 reveals a higher amount
of twins, especially compression and double twins. The
twins are concentrated along deformation bands in di-
rect correspondence to newly formed small grains.
728 K. Hantzsche et al. / Scripta Materialia 63 (2010) 725730
Figure 3. Textures of binary MgRE sheets: (a) recalculated (0 0 0 2)-
pole gures of sheets with a low and high alloying content in as-rolled
condition and after annealing; (b) maximum (0 0 0 2)-pole gure
intensity in as-rolled condition and (c) after annealing (accuracy of the
texture measurements is 0.2.).
Figure 4c and d shows the number fractions of mis-
orientation angles for both sheets. In Figure 4c a domi-
nant misorientation angle of 30 appears, which is
typically found for magnesium sheets with a strong tex-
ture. A corresponding number of tensile twins is likely to
cause a higher number fraction of misorientations be-
tween 85 and 90. In Figure 4d the distribution of mis-
orientation angles between grains appears quite
dierent. In particular, larger misorientation angles are
more signicant and peak number fractions are found
at orientations that correspond to compression twins
(e.g. 56 for {1011}-twins and 64 for {1013}-
twins) and double twins (i.e. 22 for {1013}/{10
12}-twins and especially 38 for {1011}/{1012}-
twins). The observed distribution of grain misorienta-
tions accounts for the weak texture of this sheet.
4. Discussion
The development of a texture during rolling of mag-
nesium alloys typically leads to a strong alignment of
basal planes in the sheet plane as a result of hot working.
This is well explained by the preference for basal slip
and twinning during the working of magnesium alloys
[19]. Strain-hardened sheets that reveal a partly recrys-
tallized but deformed microstructure tend to exhibit
strong basal textures that weaken signicantly if a fur-
ther heat treatment is applied (e.g. [20]). A well-recrys-
tallized sheet from alloy AZ31, however, tends to
strengthen its texture again if exposed to heat treatment
that can lead to an overall grain growth: this is also fre-
quently observed for cubic metals and alloys [21]. The
same behaviour is found in this study for pure magne-
sium and for binary alloys containing only a very small
amount of RE element. Such grain growth is likely to
cause growth selection of grains with the predominant
orientation of basal planes in the sheet plane. For those
alloys of this study that contain a higher amount of Ce,
Nd or Y, two major dierences are observed: (i) weak
textures appear already in the as-rolled state; and (ii) a
further weakening of these textures is caused by heat
treatment. These results are connected with two major
changes in the microstructure:
(1) Sheets with a high content of RE elements show a
larger number of compression and double twins than the
sheets with a low RE content in the as-rolled condition.
It is notable that these twins are mainly found in defor-
mation bands in close proximity to newly formed grains.
These twins apparently contribute to the development of
orientations in the overall weak texture. Cottam et al.
[22] observed that the texture of newly nucleated,
dynamically recrystallized (DRX) grains does not essen-
tially change the original texture of unrecrystallized par-
ent grains in MgY alloys. This supports the assumption
that new orientations formed by twins in the deforma-
tion bands persist in neighbouring new DRX grains
and therefore contribute to the texture development of
the sheet. The signicance of these orientations in the
overall texture is then related to the grain growth mech-
anisms during a subsequent heat treatment.
It has also been noted by Cottam et al. [22] that the
deformation texture changes at higher Y content, which
they related to an increasing activity of <c + a> slip. In
addition, Agnew et al. [23] showed that the balance of
deformation mechanisms during plastic deformation
can be changed by alloying, e.g. with Y or Li. In sum-
mary, a change in the activity of deformation mecha-
nisms is known to occur and is likely to change the
texture of the sheets.
(2) All annealed sheets are completely recrystallized
and changes in the microstructure can be related to
grain growth. The average grain size of the sheets de-
creases with increasing element content and therefore
with increasing concentration of the element in solid
solution or amount of precipitates. Such a grain growth
restriction accompanied by texture weakening is consis-
 K. Hantzsche et al. / Scripta Materialia 63 (2010) 725730
Figure 4. EBSD orientation maps in as-rolled condition with highlighted twin boundaries (red: {1012}-tensile twins; blue: {1011}- and {1013}-
compression twins; yellow: {1011}/{1012}- and {1013}/{1012}-double twins): (a) MgNd0.01; (b) MgNd0.04; and corresponding misorientation
angles: (c) MgNd0.01; (d) MgNd0.04.
tent with grain boundary pinning eects caused by sol-
ute segregation or particles.
It is worthwhile to note that both eects described
above were repeated in all passes throughout the entire
rolling process, nally leading to a weak sheet texture.
5. Summary
This study conrms that magnesium sheets with weak
textures are achievable by using alloying elements such
as Nd, Ce and Y. The amount of the RE addition re-
quired for sucient texture weakening is connected with
the solid solubility of the respective element. Such weak
textures promise improved sheet formability [3]. The
weakening of the texture is connected with the appear-
ance of deformation bands containing twins and the
restriction of grain growth. The observed deformation
bands with twins dier from typical macroscopic shear
bands generated by severe inhomogeneous deformation.
The latter bands tend to initiate cracks during sheet-
forming processes and therefore lead to a decrease in
formability [24].
Acknowledgements
The authors appreciate the intense and valuable dis-
cussions on many aspects of this paper with Sean Agnew
729
and Jason Hadorn at the University of Virginia, Char-
lottesville, VA, USA. The authors appreciate the
nancial support of this study by the Deutsche Fors-
chungsgemeinschaft (Grant Nos. KA 1053/10-1 and LE
1395/3-1) as part of the World Materials Network.
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