Influence of Rolling Conditions
Tensile tests at room temperature were con-
on the Microstructure and
Mechanical Properties
of Magnesium Sheet AZ31
By Frank Kaiser,* Jan Bohlen, Dietmar Letzig,
Karl-Ulrich Kainer, Andrezej Styczynski, and
C. Hartig
The main reason for using lightweight metals in the auto-
motive industry is the potential saving of natural energy re-
sources simply by weight reduction. Magnesium, as the light-
est available construction metal, offers a wide range of
opportunities for use in automobiles. At present mostly cast
parts are used and the use of wrought magnesium alloys is
still well below the potential.[1] There are two main reasons
for this: a lack of sufficient cold formability and the anisotro-
py of the properties of the finished sheets.[2,3] Also, the rolling
process is not adequately developed and still needs a lot of
improvement to produce material with the required proper-
ties.
Generally, mechanical properties are affected by grain size,
microstructural homogeneity, and texture.[4] In a plastic de-
formation process such as rolling, the process parameters
cause changes in the microstructure, which determine the
mechanical properties. It is important to understand the com-
plex mechanisms of deformation, recovery, and recrystalliza-
tion during plastic deformation at elevated temperatures in
order to achieve process development.[5]
This Communication describes two aspects of the defor-
mation behavior of magnesium sheets. First, we give a brief
mechanical characterization of a commercial magnesium with
a focus on the anisotropy and the possible microstructural
causes of this behavior. Second, we discuss the rolling process
and its influence on the sheets. The aim is to show the influ-
ence of the parameters on the microstructure and texture and
how this could affect the anisotropy in the rolled sheets.
Experimental: We examined commercial rolled sheet, and
specimens rolled to 3 mm thickness in our laboratory from
various starting materials. Commercial AZ31B rolled sheet
(with nominal composition 3 wt.- % Al, 1 wt.- % Zn, balance
Mg) was provided in the stress-relieved H24 temper and
± ity, though the strain is slightly greater, on average, for TD.
[*] F. Kaiser, Dr. J. Bohlen, Dr. D. Letzig, Prof. K. U. Kainer
GKSS Research Center GmbH
21502 Geesthacht (Germany)
E-mail: frank.kaiser@gkss.de
Dr. A. Styczynski, Dr. C. Hartig
Technical University Hamburg±Harburg
21073 Hamburg (Germany)
ADVANCED ENGINEERING MATERIALS 2003, 5, No. 12 DOI: 10.1002/adem.200300404
1.6 mm thick.
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ducted on a Zwick Z050 universal testing machine with a
constant strain rate of 10±3 s±1. The commercial sheet tensile
samples were 125 mm ” 20 mm ” 1.6 mm in size; samples
taken from our rolled material had a cross section of 3 mm ”
6 mm. Owing to the limited material available, the specimen
shape was freely chosen, taking the standard ISO specifica-
tions into consideration. Texture was measured by X-ray dif-
fraction in reflection geometry on a Brukers AXS diffractome-
ter.[6,7] Metallography was performed after picric acid
etching.
A laboratory mill was used for all rolling experiments. The
rollers were kept at room temperature and operated at a
speed of 3 m/min rolling rate. The specimens for stepwise
rolling had a size of roughly 100 mm ” 50 mm ” 10 mm (l0 ”
b0 ” h0). The specimens for one-step rolling experiments had
different starting dimensions in order to reach a final sheet
thickness of 3 mm. All rolling was done at a specimen tem-
perature of 400 C on withdrawal from the furnace, which
was located directly next to the mill.
The first part of the experimental processing consisted of
stepwise rolling by reducing the thickness in logarithmic steps
of 0.1. For this experiment two different feedstocks were com-
pared: AZ31 sheet and a specimen of the same alloy produced
by continuous casting. After every five steps a sample was tak-
en from the rolled material (after air-cooling) and kept for
further analysis. The remaining material was annealed for
20 min in order to control the material temperature before
further rolling. It was additionally treated for 2 min between
rolling passes. Thus the rolling process produced thin sheets
up to a final reduction in thickness of 86 % (r = 2; r = ln h/h0).
For the second part of the experiment, AZ31 continuous-
cast specimens were rolled at 400 C, but this time in one step
directly down to a final sheet thickness of h = 3 mm, r = 0.17
(16 %) to 1.05 (65 %). The material was solution annealed for
10 h before rolling to avoid any influence from precipitation,
and water-quenched after rolling.
Results: Tensile tests at room temperature gave the me-
chanical properties of yield strength (YS) and tensile strength
(UTS) as a function of sheet orientation. For these tests, speci-
mens were taken from the sheet at 0 and 90, where 0 means
the rolling direction (RD) and 90 indicates the transverse di-
rection (TD). Figure 1 clearly shows the high dependence of
YS and UTS on the orientation of the sheet. The difference in
YS between RD and TD (DYS) is more than 50 MPa, which is
roughly 20 % of the maximum value at TD. UTS is less aniso-
tropic. There seems to be no great effect of direction on ductil-
For the heat treatments, 1.6 mm RD and TD specimens
were used; they were heated for 30 min in a standard forced-
air furnace. Afterwards, tensile tests were carried out at room
temperature. DYS drops to about 30 MPa for the 200 C heat
treatment temperature (Fig. 2). This difference remains al-
most constant for higher heat treatment temperatures. The
anisotropy of the tensile strength follows the same pattern,
Ó 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 891
COMMUNICATIONS

350 a) b)
a)
300
Engineering Stress [MPa]

250
Transverse Direction

200 Rolling Direction

150

100

50

c)
0
0 5 10 15 20 25
Engineering Strain [%]
Fig. 1. Stress±strain curves for rolling direction and transverse direction, tests at RT
and e_ = 10±3 s±1.

80

70

60

50
∆YS [MPa]

Fig. 3. a) Continuous cast sample, b) rolled sample, c) cracks at high reduction ratio.
40

30
homogeneously rolled part. The same applies to samples for
20 texture measurements. At higher deformation rates the edges
were severely cracked, approximately 5±20 mm towards the
10
sheet center (Fig. 3). Figure 4 shows the results of the tensile
0 tests at 16, 44.5, and 65 % reduction in sheet thickness. Except
0 20 50 100 150 200 250 300 350 400 450 500 550
for the TD specimen at 65 %, yield strength and maximum
As-Received / Heat Treatment Temperature [ºC]
strength increase with increasing amount of rolling. In RD
Fig. 2. Yield anisotropy illustrated by DYS as a function of testing temperature.
the specimens are brittle, they break at very low strains and
sometimes hardly reach the YS. The TD specimens are more
but the differences are smaller at first and can be neglected ductile, still the values are usually below 4 % strain other than
with increasing heat treatment temperature. the 16 % sample, which shows almost 8 % elongation to frac-
Tensile test specimens were taken from each rolled sample ture. All the tests show that the elongation to fracture is great-
in both RD and TD. As far as possible, the specimens were er for TD than RD, which is contrary to the results from the
taken from the center of the sheet in order to get the most commercial sheet. DYS is about 60 MPa at 16 % deformation

a) b) c)
300 300
300

250 250
250

200
Stress [MPa]

200 200
Stress [MPa]
Stress [MPa]

150 150 150

100 100 100

50 rolling direction 50 rolling direction

50 rolling direction transverse direction
transverse direction
transverse direction 0 0
0 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
0 1 2 3 4 5 6 7 8
Strain [%] Strain [%]
Strain [%]
Fig. 4. Stress±strain curves from sheet specimens rolled with: a) 16 %, b) 44.5 %; c) 65 % degree of rolling. Tests at RT and 10±3 s±1.

892 Ó 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim http://www.aem-journal.de ADVANCED ENGINEERING MATERIALS 2003, 5, No. 12
Kaiser et al./Influence of Rolling Conditions on the Microstructure and Mechanical Properties

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a)

350

300
Yield Stress MPa

250

200

150

100 Fig. 7. Pole figures of the (0002) and (101Å0) planes (250 C).

50 transverse direction
rolling direction
(0002) basal plane orientation distribution of the heat treated
0
0 10 20 30 40 50 60 70 80 sheet drops about 25 % and is more centered compared to the
original state.
Degree of Rolling %
For the cast materials, the texture of the feedstock shows
b)
random orientation and is therefore illustrated only for the
350
gravity-cast material. Figure 8 shows that for multi-rolled
castings the preferred orientation of the basal planes does not
300 show an offset. Figure 9 shows that the one-step rolled sam-
Tensile Stress MPa

250 ples show the typical double peak, though with unequal in-
tensity. Another distinctive feature is the distribution of the
200
planes in TD, which is nonexistent in the other materials. The
150

100

50 transverse direction a)
rolling direction
0
0 10 20 30 40 50 60 70 80
Degree of Rolling %
Fig. 5. a) YS, b) UTS of rolled sheet.

and goes down to 25 MPa at 44.5 %. The results for the mate-
rial rolled at 65 % are different: DYS is just over 100 MPa. The
loss of strength, especially for TD, is supposedly an effect of
dynamic recovery and recrystallization. The mechanical
b)
properties are given in Figure 6.
The textures were measured for the commercial 1.6 mm
sheet in the as-received condition. Figure 7 shows the (0002)
basal plane pole figure and the (101Å0) prismatic plane pole
figure for this feedstock; Figure 8 represents the correspond-
ing pole figures for the 250 C heat treated material. The basal
plane pole figures show a preferred orientation of the (0002)
plane for both conditions, the prismatic planes show no pre-
ferred orientation for either condition. It is clear that the
c)

Fig. 8. Pole figures for gravity cast sample: a) as-received; b) u = 35.9 %; c) u = 62.5 %
Fig. 6. Pole figures of the (0002) and (101Å0) planes (as-received condition). (400 C, multiple step rolling).

ADVANCED ENGINEERING MATERIALS 2003, 5, No. 12 http://www.aem-journal.de Ó 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 893
 Kaiser et al./Influence of Rolling Conditions on the Microstructure and Mechanical Properties

(101Å0) prismatic plane distribution shows no significant con-

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a)
spicuity in comparison.
Optical microstructure investigations were carried out on
the 1.6 mm heat treated sheets and the rolled samples to char-
acterize the evolution of the grain size with rising tempera-
ture and increasing amount of deformation (Fig. 10).
The grain size distribution of the commercial sheet in its
as-received condition is very inhomogeneous. The feedstock
consists of grains full of twins; visible grains are 20 lm on
average, some as large as 60 lm. The heat-treated specimen is
b) free of twins, the grain size is about 5 lm. The decrease in the
grain size after heat treatment is probably because the micro-
structure of the as-received condition is hardly identifiable.
The gravity-cast material shows an average grain size of
1800 lm. The rolled sheets have grains of 10±15 lm after a
deformation of u » 1 (» 63 %), which is comparable to the
commercial sheet. While the average grain size of 350 lm
could be observed with the continuous-cast feedstock sample,
only the minor deformed rolled samples show a visible grain
structure. Beyond 50 % deformation, one can see highly de-
c) formed grains, which form some typical bands throughout
the specimen oriented along RD (Fig. 11). In some areas the
beginning of dynamic recrystallization (DRX) can be ob-
served. The new grains have sizes below 1 lm.
Discussion: In previous investigations it was concluded
that the strongly anisotropic behavior of commercial AZ31
magnesium sheet is due to the strong rolling texture of the
material.[8,9] It was assumed that the slightly egg-shaped' dis-
tribution of the (0002) basal plane has a significant influence
on the planar anisotropy of the sheet. This means that there is
Fig. 9. Pole figures for slab cast sample: a) 16 %; b) 44.5 %; c) u = 65 % (400 C, sin-
a higher probability of the activation of slip systems accord-
gle step rolling). ing to the Schmid factor along RD than for TD.

a) c) e)

b) d)

Fig. 10. a) Commercial sheet in as-received condition; b) heat treated at 250 C for 30 min; c) gravity casting as received; d) rolled gravity casting; e) continuous cast material in
as-received condition: rolling direction facing to top.

894 Ó 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim http://www.aem-journal.de ADVANCED ENGINEERING MATERIALS 2003, 5, No. 12
Kaiser et al./Influence of Rolling Conditions on the Microstructure and Mechanical Properties
Fig. 11. Micrographs of the continuous cast rollings with deformation of: left) 16 %; middle) 44.5 %; right) 65 %. Material rolled in a single step at 400 C; images show cross sec-
tion, rolling direction facing to top.
The change from the typical off-set-peak texture to a cen-
tered distribution for the heat treated sample must influence
the anisotropy. The tensile tests clearly show the decreasing
anisotropy of yield, suggesting that the single-peak texture
will result in lower anisotropy. The recovery of the micro-
structure also seems to have a positive effect on the activation
of deformation mechanisms, thus hardening effects cannot be
neglected and need to be discussed further.
The single-pass and multi-pass rolling experiments com-
pare a fairly simple process without any static recrystalliza-
tion on the one hand, and a complex thermomechanical treat-
ment on the other side. Since the commercial sheet was also
subject to a complex thermomechanical treatment with inter-
annealing, a direct comparison of the sheet and its resulting
mechanical properties with the multi-step rolling experiments
is justifiable. The results confirm this comparison; the texture
of the multi-pass experiments is very similar to the texture of
the heat-treated commercial sheet (Fig. 7 and Fig. 8). In both
cases, the (0002) basal texture shows the clearly zoned ªegg-
shapedº distribution with a longish peak in the sheet layer
and also the peak intensities are at close quarters.
The basal textures of the one-step rolling experiments
show that the double peak is a result of the rolling process, in-
dependent of recrystallization. Simulation results show
[101Å0] texture development. Taking this into consideration,
the basal texture of the commercial sheet seems logical, since
the H24 condition describes a final cold rolling step with a
subsequent short annealing. The microstructure of the sheet
with its many twins confirms this. Therefore, one could as-
sume that the off-set-peak is a state between the double-peak
texture and centered single-peak distribution.
As a consequence, the mechanical properties of the one-
pass rolled sheet would be expected to show similar results
to the commercial sheet, namely higher YS in TD. As shown
in Figure 4, this is not the case: the converse is true.
At this point it becomes necessary to include the distribu-
tion of the Euler angles in TD. Unlike the multi-pass rollings
there is a significant spread of basal planes in TD at higher
ADVANCED ENGINEERING MATERIALS 2003, 5, No. 12
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deformation rates, which adds to the formation of the double
peak. Additionally it must be borne in mind, that rolling at
different reduction ratios leads to a completely different hard-
ening behavior of the material, compared with a process that
includes interannealing.
Summary: Tensile tests were carried out on a commercial
AZ31 sheet of 1.6 mm thickness in order to investigate the an-
isotropy of the mechanical properties, especially the yield.
Tests at RT show a strong vertical and planar anisotropy of the
sheet, which was explained by the strong rolling texture. Ex-
periments with heat-treated specimens lead to a decrease in
anisotropy of yield of about half its corresponding value at RT.
Rolling experiments with single-pass and multi-pass roll-
ing with annealing between the steps were conducted at
400 C. The results indicate that annealing between the rolling
steps leads to a concentric basal plane distribution, whereas a
single-pass rolled specimen shows a typical double peak tex-
ture. This suggests that the double peak texture is a pure de-
formation texture. The assumption that this texture will result
in similar or greater anisotropic behavior compared with a
rolled and interannealed material was not demonstrated.
Tensile results from specimens taken from the single-pass
rolled material show an opposite anisotropy with the rolling
direction being stronger than the transverse direction.
Further investigations are required, to give more informa-
tion on the mechanisms of anisotropy and its relationship with
texture and microstructure. Upcoming work needs to analyze
the influence of texture on the mechanical properties more
closely. It must also take the effect of hardening of the material
into consideration in order to better predict the behavior of
magnesium sheets in terms of commercial sheet production.
Received: September 15, 2003
±
[1] K. U. Kainer (Ed.), Magnesium Alloys and their Applica-
tions, Wiley-VCH, Weinheim 2000.
[2] E. F. Emley, Principles of Magnesium Technology, Perga-
mon, Oxford 1966.
http://www.aem-journal.de Ó 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 895
 [3] A. Beck, Magnesium und seiner Legierungen, Springer,
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Heidelberg 1939.
[4] U. F. Kocks, in Texture and Anisotropy, (Eds: U. F. Kocks,
C. N. TomØ, H. R. Wenk) Cambridge University Press
1998.
[5] J. Bohlen, A. Horstmann, F. Kaiser, A. Styczynski,
D. Letzig, K. U. Kainer, in Magnesium Technology: Proc.
TMS Ann. Mtg., Seattle, 2002 (Ed.: H. I. Kaplan), TMS,
Warrendale, PA 2002, p. 253.
[6] A. Styczynski, Ch. Hartig, J. Bohlen, D. Letzig, Scripta
Mat. 2003, in press.
[7] V. Kree, J. Bohlen, D. Letzig, K. U. Kainer, Prak. Metal-
logr. 2003, in press.
[8] S. R. Agnew, in Magnesium Technology: Proc. TMS Ann.
Mtg., Seattle, 2002 (Ed.: H. I. Kaplan), TMS, Warrendale,
PA 2002, p. 169.
[9] F. Kaiser, D. Letzig, J. Bohlen, A. Styczynski, C. Hartig,
K. U. Kainer, Mater. Sci. Forum 2003, 419±422, 315.
General Corrosion and Galvanic
Corrosion Properties of
differently PVD treated
Magnesium Die Cast Alloy
AZ91**
By Holger Hoche,* Carsten Blawert,
Erhard Broszeit, and Christa Berger
Although the load bearing capacity of magnesium alloys is
quite low in comparison to other construction materials, in-
vestigations of the authors showed good wear properties of
PVD-CrN coated magnesium die cast alloy AZ91. In a certain
parameter field the wear properties were in the same range
as for PVD-CrN coated steel or titanium alloys.[1] Unfortu-
nately the CrN coated specimens failed the corrosion tests
due to crucial galvanic corrosion between the metalloid CrN
and the less noble magnesium.[2]
± nesium alloys for moving parts by ensuring a sufficient wear
[*] H. Hoche, Dr. E. Broszeit, Prof. C. Berger
Staatliche Materialprüfungsanstalt und Fachgebiet und
Institut für Werkstoffkunde
Technischen Universität Darmstadt
D-64283 Darmstadt
E-mail: hoche@mpa-ifw.tu-darmstadt.de
C. Blawert
GKSS Forschungszentrum Geesthacht GmbH
D-21502 Geesthacht
[**] The authors acknowledge the financial support by the DFG
(Deutsche Forschungsgemeinschaft).
896 Ó 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim DOI: 10.1002/adem.200300402
Developing PVD coating systems with better corrosion re-
sistance leads to a duplex process, consisting of a PVD-plas-
ma anodisation and an Al2O3 top coating which can both be
performed in a modified commercial PVD unit. Even in the
area of specific coating failures (Vickers indentations and
scratches) the duplex coatings are not more affected by corro-
sion than the overall surface.
Because the corrosion properties are not completely clari-
fied yet, the aim of this work is to contribute to their scientific
description. The following PVD-coating systems are included
in the studies, which all meet the conditions of an acceptable
wear resistance.
[1]
l 9 lm CrN hard coating
l 3 lm TiN hard coating
l 0.5 lm plasma anodisation layer and 3 lm Al2O3 coat-
ing.[2]
Information about the general corrosion properties of the
above mentioned coating systems is gathered with electro-
chemical current versus Potentials measurements. The tested
specimens were investigated by means of optical microscopy,
SEM and EDX. Furthermore a novel immersion technique to
determine the time dependent corrosion behavior of coated
magnesium alloys is introduced.[3] The galvanic corrosion
properties were tested according to DIN 50919. The speci-
mens were tested in 3 % NaCl solution and as contact materi-
als the aluminium alloys AlMgSi0.5 and AlSi9Cu3 and a roll-
er bearing steel 100Cr6 were used. The tested specimens from
the immersion tests and the contact corrosion tests were in-
vestigated with optical microscopy.
The care of brief resources and the economical use of pri-
mary energies are one of the great political and technological
challenges of this new century in order to lower emissions
and to reduce the increasing environmental pollution. Con-
cerning this background, magnesium seems to be very pro-
spective to fulfil these demands. Besides its high strength/
weight ratio, magnesium alloys combine the demands of
good castability, good machiniability and a great recycling
potential.[4] Because the resources of magnesium in the
oceans and in the earth's crust are nearly inexhaustible mag-
nesium presents an ecological useful alternative to plastics.
Because of the bad wear properties of magnesium alloys
their application is limited up to now to the static component
field. However, a considerably higher potential for the lasting
fuel and emission reduction could be the application of mag-
resistance, e.g., with PVD hard coatings.
Extensive research of the authors in deposition of reliable
PVD hard coatings on magnesium alloys,[1,2,5,6] showed com-
parable wear results in a certain parameter field in compari-
son to PVD coated titanium- and iron-based alloys. Consider-
ing the demands for the application of magnesium alloys in
tribological systems the corrosion problematic becomes of
crucial importance, particularly due to the PVD process re-
lated pinholes which can lead to crucial corrosion. If one
thinks of decorative PVD coatings a reliable corrosion protec-
tion of the magnesium surface for applications in aggressive
ADVANCED ENGINEERING MATERIALS 2003, 5, No. 12