Scripta Materialia 48 (2003) 647652

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Crystallography of Mg17Al12 precipitates in AZ91D alloy

M.-X. Zhang *, P.M. Kelly
Division of Materials, School of Engineering, University of Queensland, St. Lucia, Brisbane, QLD 4072, Australia
Received 2 April 2002; accepted 21 August 2002

Abstract
Kikuchi diraction was used to accurately determine the orientation relationship (OR) between Mg17 Al12 precipitates and matrix in an AZ91D alloy. For both continuous and discontinuous precipitations, the Burgers OR and the
Potter OR were equally observed. The lattice parameter of Mg17 Al12 associated with the former is bigger than that of
the latter.

2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.
Keywords: Crystallography; Electron diraction; Microstructure; Magnesium alloy

1. Introduction
AZ91 (Mg9wt.%Al0.51.0wt.%Zn0.3wt.%
Mn) is the most popular magnesium alloy due to
its superior combination of castability, mechanical
strength and ductility. Previous work [111] has
shown that the Mg17 Al12 intermetallic compound
(b phase) is the only precipitate generated during
ageing after solution treatment. This precipitation
can occur either continuously (general) or discontinuously (cellular). In both cases the precipitations are in lamellar form [111]. These two
precipitation reactions take place competitively
and simultaneously over a wide range of ageing
temperature [1,2]. Continuous precipitation occurs
through nucleation and growth of individual phase

*
Corresponding author. Tel.: +61-7-3365-3669; fax: +61-73365-3888.
E-mail address: m.zhang@minmet.uq.edu.au (M.-X. Zhang).

particles within the parent grains and leads to a

progressive change in matrix composition [1,8].
Discontinuous precipitation is nucleated on grain
boundaries and grows as nodules [1,5,6,8]. Although the maximum solubility of Al in Mg is up
to 12.5wt.%, the precipitation hardening eect of
b phase in MgAl based alloys is small [13]
compared with other alloys. Clark [1] and Crawley
and Lagowski [2,3] considered that this is due
to the unfavourable orientation of b platelets
to block basal slip and the large inter-precipitate
spacing. Hence, to completely understand the
mechanism of precipitation hardening and to seek
ecient means for improving the strength of Mg
Al based alloys, it is essential to study the orientation relationship (OR) between b phase and
matrix.
For both continuous and discontinuous precipitates, the previously reported predominant OR
between the b phase, which has BCC (B) structure
and the HCP Mg matrix (H) in MgAl based
alloys is the Burgers OR [2,3,8,9,11].

1359-6462/03/$ - see front matter
2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.
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M.-X. Zhang, P.M. Kelly / Scripta Materialia 48 (2003) 647652

The Burgers OR:

0 0 0 1H k0 1 1B ;

2

1

1 0H k1

1 1B

Precipitates with this OR is parallel to the basal

plane of matrix, i.e., the habit plane is (0 0 0 1)H . In
addition, Duly et al. [5] reported that the Potter
OR was occasionally observed.
The Potter OR:
0 1

1 1H k1 1 0B ;

0 0 0 1H 2 from 0 1 1B ;
1 1B
2

1

1 0H k1

Other ORs were also observed in MgAl based

alloys. For the precipitates that lie perpendicular
to basal plane, three ORs were reported [3,9,12].
stmoe (GO) OR:
The Gj
onnesO
0 0 0 1 k0 1 1 ; 1 1

2 0 k2 1

1
H

The Porter OR:

1

1 2 1H k0 1 1B ;

1

1 0 0H k0

1 1B

The Crawley OR:

0 0 0 1H k1

1 1B ;

1 0

1 0H k1 1 0B ;

1

2 1 0H k

1 1 2B
Precipitate following these ORs lies on the prism
plane of the Mg matrix with the habit plane of
f1
1 0 0gH .
All the above ORs were determined using
conventional selected area diraction techniques,
which is often not accurate enough to distinguish
small dierences, such as the 1.93 rotation about
2
1

1 0H k1

1 1B that distinguishes the Burgers OR
from the Potter OR. In addition, the eect of
variations in chemical composition of the b phase
on its lattice parameters and OR is important.
Hence, the aims of the present work are

to investigate the orientation dierence between

individual precipitates in a single grain.

2. Experimental
As cast commercial AZ91D alloy (9.0wt.%Al
0.7wt.%Zn0.13wt.%Mn) was used in the present
work. 15  15  10 mm block specimens were solution treated at 413 C for 16 h followed by water
quenching. Specimens were then aged at 350 C for
6 h or at 168 C for 16 h. Another specimen was
furnace cooled after solution treatment. For both
the solution treatment and the subsequent ageing,
specimens were buried in a mixture of 80% foundry sand and 20% coke (in volume) to minimize
the oxidation of specimens. Experimental results
showed that this simple method eectively reduced
oxidation of the specimens.
The preparation process for TEM specimens
was as follows. Block specimens were slowly cut
into 0.81.0 mm slices using a diamond-cutting
blade. After mechanical grinding to 0.080.1 mm
thick thin foil, 3 mm in diameter discs were punched from the foil. The discs were then jet polished
in a solution of 10.6 g lithium chloride, 22.32 g
magnesium perchlorate, 1000 ml methanol and
100 ml 2-butoxy-ethanol at )55 C with voltage of
8090 V. Jet polishing was stopped just before
perforation, and followed by ion milling thinning
to form a hole. All thin foils were immediately
examined in a JEOL 4010 or JEOL 2010 TEM.
ORs were determined using convergent beam
Kikuchi line diraction patterns [13,14]. The habit
plane of each precipitate was determined using the
trace width [15] and the lattice parameters of individual precipitates were determined from Kikuchi pattern by the technique described in [16].

3. Results and discussion

to use convergent beam Kikuchi line diraction
patterns to accurately determine the ORs between b phase and matrix [13,14];
to determine the habit plane of the precipitates
[15];
to study the eect of lattice parameters of b
phase on the OR, and

3.1. Morphology of Mg17 Al12 precipitates

The micrographs of Mg17 Al12 precipitates in
AZ91D alloy after solution treatment followed by
furnace cooling, ageing at 168 and 350 C are
shown in Fig. 1. In specimens aged at 168 C for

M.-X. Zhang, P.M. Kelly / Scripta Materialia 48 (2003) 647652

649

Fig. 1. Morphology of b precipitates in AZ91D after solution treatment at 413 C for 16 h and (a), (b) aged at 168 C for 16 h; (c) aged
at 350 C for 6 h and (d) continuously cooling in furnace.

16 h, discontinuous precipitation is the dominant

morphology, as shown in Fig. 1a. The precipitates
have a lamellae morphology (Fig. 1b). After ageing at 350 C for 6 h, the majority of the microstructure is continuous precipitation accompanied
by a small amount discontinuous precipitation
near the grain boundaries (Fig. 1c). After furnace
cooling, the whole specimen consists of the pearlite-like continuous precipitation (Fig. 1d).
The morphology in Fig. 1 is consistent with
previous reported results [1,4,7], in which the continuous and discontinuous precipitation occurs
competitively. Dulys work [7] indicated that
continuous precipitation is favoured at high temperatures, whereas discontinuous precipitation
dominates at intermediate temperatures. Hence,
after ageing at 350 C the continuous precipitation
is the dominant morphology. According to Dulys
work [7], ageing at 168 C should lead to the
mixture of continuous and discontinuous precipitation. However, because discontinuous precipita-

tion occurs from grain boundaries [1,4,7,17], which

is easier than intragranular precipitation for continuous precipitates, discontinuous precipitation
should take place rst at this temperature. In addition, 16 h ageing is not long enough to produce
continuous precipitation. Thus, only discontinuous
precipitates were observed. For the continuously
furnace cooling process, as continuous precipitation has invaded the whole specimen at high temperatures before any discontinuous precipitation
could occur at lower temperatures, almost full
continuous precipitates were observed as shown in
Fig. 1d.
3.2. Crystallography of Mg17 Al12 precipitates
For both continuous precipitation (aged at
350 C and furnace cooling) and discontinuous
precipitation (aged at 168 C), there was no signicant dierence in both OR and habit planes.
Two major ORs between b phase and matrix have

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M.-X. Zhang, P.M. Kelly / Scripta Materialia 48 (2003) 647652

Fig. 2. Enlarged regions of stereographic projection (in terms of [0 0 0 1]H ) showing the Burgers OR and the Potter OR between the
b phase and matrix in AZ91D alloy: (a) near 2
1
1 0H showing the position of 1
1 1B for both ORs (b) near (0 0 0 1)H showing the
position of (0 1 1)B for both ORs.

been observed. They are the Burgers OR and the

Potter OR. The collected experimental results,
together with the Burgers OR and the Potter OR,
are shown in Fig. 2. These gures are the enlarged
regions of stereographic projection in terms of
[0 0 0 1]H after transferring all the experimentally
determined ORs to the same variant. Because
2

1

1 0H is on the border of the stereographic
projection, some experimental data in Fig. 2a are
out of the normal stereographic projection. These
data should be expressed in the projection near


2 1 1 0H . But, in order to clearly show the experimental results, in which 1

1 1B is parallel to
2

1

1 0H for both the Burger OR and the Potter
OR, these experimental data are shown in the
same gure as Fig. 2a. In the total of 47 experimental observations, 24 are the Burgers OR and
23 obey the Potter OR. Both ORs are observed in
either continuous precipitation or discontinuous
precipitation. The Burgers OR was reported as the
major OR between the b phase and the matrix in
almost all of the previous work [2,3,8,9,11]. While,
the Potter OR was seldom mentioned. Only Duly
et al. [5] reported once. This is because both ORs
are very close to each other (related by a rotation
of 1.93 about 2
1

1 0H k1

1 1B ), and all the previously reported ORs were determined using conventional selected area diraction technique that is
less accurate. Hence, it is dicult to distinguish
between these two ORs. When the more accurate
Kikuchi line diraction technique is used in the
present work, the two ORs are distinguished and

both occur between the b precipitates and the

matrix in the AZ91D alloy.
The habit planes determined for both ORs are
more complicated than OR. For the Burgers OR,
90% of determined habit planes are 0 0 0 1H k
0 1 1B , which is consistent with previously
reported results [2,3,8,9,11]. The other habit
planes for this OR, namely (0
1 1 2H k2 3 1B
and (
1
2 3 0H k1 1
1B , were only observed when the
Burgers OR and the Potter OR existed within the
same matrix grain. The former has also been observed in Dulys work [5], the latter is reported for
the rst time in the present work. Although Duly
et al. [5] has reported that occasionally, the b precipitates can grow on 0
1 1 2H k2 3 1B crystallographic plane when the Potter OR is obeyed,
no unique habit planes were found in the present work. Approximately, the determined results
are close to one of the following three habit
planes within the range of 16: 1 0
1 1H k1 0 1B ,
(
1
2 3 0H k1 1
1B , and 0 0 0 1H k0 1
1B . The different habit planes indicate that the nucleation
orientation and the growth direction of the precipitations corresponding to the Potter OR is dierent
from that of the precipitations having the Burgers
OR. More detailed work is being carried out.
In order to understand more about the precipitation associated with dierent habit planes and
ORs, the lattice parameters of individual precipitates were determined using Kikuchi line diffraction patterns [16]. As expected, the lattice
parameters of individual precipitates vary from

M.-X. Zhang, P.M. Kelly / Scripta Materialia 48 (2003) 647652

1.050 to 1.069 nm. This is attributed to the variation of the chemical composition of Mg17 Al12
precipitates above 100 C, according to the MgAl
equilibrium phase diagram [18]. The lattice
parameter of the precipitates associated with
the Potter OR is 1:055 0:005 nm, and it is
1:066 0:003 nm for the precipitates that obey the
Burgers OR. This crystallographic feature of b
precipitation in AZ91D alloy can be well explained
using the edge-to-edge matching model [19],
which will be described more completely in a
subsequent paper.
In addition to the Potter OR and the Burgers
OR, the Crawley OR and the Porter OR are also
observed in the furnace cooled and 168 C aged
specimens. Unlike Cellottos ndings [9] that the
Crawley OR is associated with the precipitates that
are perpendicular to the basal plane and the Porter
OR corresponds to precipitates that lie in an angle
to the basal plane, both ORs were observed in

651

precipitates that are perpendicular to the lamellar (0 0 0 1)H major precipitates, which obey the
Burgers ORs. The determined habit plane for
both ORs is identical. It is (
1 0 1 0H k0 1 1B , which
is consistent with Cellottos result for the precipitates that are perpendicular to the basal plane and
obey the Crawley OR [9]. Precipitates that lie in an
angle to the basal plane have never been observed
in the present work.
3.3. Precipitation orientation within one matrix
grain
Previous work [8,9] has indicated that from the
symmetry properties of both Mg matrix and b
phase related by the Burgers OR, there are six
equivalent variants of the Burgers OR. Because the
Potter OR can be generated by a rotation of 1.93
about h2
1
1 0iH kh1
1 1 iB , it also has six equivalent variants. Rotating the Burgers OR about

Fig. 3. (a) Typical TEM micrograph of b precipitates; (b) Kikuchi patterns from matrix; (c) Kikuchi pattern from precipitate-A
showing the Burgers OR; (d) Kikuchi pattern from precipitate-B showing the Potter OR.

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M.-X. Zhang, P.M. Kelly / Scripta Materialia 48 (2003) 647652

2
1

1 0H k1

1 1B axis to the 0 1

1 0H direction gives
rise to the OR: 0
1 1 1H k1 1 0B , 2

1

1 0H k1

1 1B .
Rotating to the opposite direction leads to another
variant of the Potter OR: 0 1

1 1H k

1 0 1B ,






2 1 1 0H k1 1 1B . Similarly, Rotation of the Burgers OR about

12

1 0H k1

1 1B and

1

1 2 0H k1

1 1B
can generate other four variants of the Potter OR.
Namely,
1 0

1 1 k1 1 0


12

1 0 k1

1 1 ;
H

1 0 1B


1 0 1 1H k

12

1 0H k1

1 1B ;

1 1 0 1H k1 1 0B

1

1 2 0H k1

1 1B ;

1

1 0 1H k

1 0 1B

1

1 2 0H k1

1 1B ;

Duly et al. [8] and Cellotto [9] have demonstrated

the dierent orientations of b precipitates that obey
the Burgers OR with matrix within one grain
in TEM observed along [0 0 0 1]H direction. In the
present work, Kikuchi line diraction patterns were
used to examining the orientations of individual
precipitates within a single grain for both continuous and discontinuous precipitations. Except different variants of the Potter OR were observed,
both the Burgers OR and the Potter OR can exist in
the same grain. Fig. 3 shows the typical TEM micrograph of b precipitation in AZ91D alloy and the
corresponding Kikuchi line diraction patterns
showing the Burgers OR and the Potter OR.
From these experimental results it can be argued that the nucleation and growth of individual
precipitates are independent on each other. The
dominant factor for determining the orientation
relationships and habit planes may be the intrinsic
crystallographic features of the two phases, such as
the close packed planes and directions [9]. More
detailed discussion will be given in a later paper.

4. Summary
1. The morphology of AZ91D alloy aged at 168
C for 16 h is dominated by discontinuous precipitation; continuous furnace cooling from solution treatment temperature leads to majority
of continuous precipitation; and both types of
precipitation can be observed when samples
are aged at 350 C for 6 h.

2. The Burgers OR and the Potter OR are the two

major OR between b phase and matrix for both
the lamellae continuous and the discontinuous
precipitations in AZ91D alloy. The major habit
plane associated with the Burgers OR is
0 0 0 1H k0 1 1B . The habit planes for the Potter OR are more complicated. They are within
19 of 1 0
1 1H k1 0 1B , 20
1
2 3 0H k1 1
1B
and 0 0 0 1H k0 1
1B .
3. The lattice parameter of the precipitates that
obey the Burgers OR is 1:06640 0:003 nm; it
is 1:05476 0:005 nm for the precipitates that
follow the Potter OR.
4. The orientations of the precipitates within one
single matrix grain may be dierent. They may
obey either dierent variants of the Burgers
OR or the Potter OR or both.

Acknowledgements
The authors are grateful for an Australian Research Council Large Grant for funding support.

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