PERGAMON Micron 32 (2001) 865±870

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A TEM study of precipitation in Al±Mg±Si alloys

J.Y. Yao a,*, D.A. Graham a, B. Rinderer b, M.J. Couper b
a
CRC for Cast Metals Manufacturing (CAST), The University of Queensland, Brisbane, QLD 4072, Australia
b
Comalco Research & Technical Support (CRTS), Comalco Aluminium Ltd., Thomastown, VIC 3074, Australia

Abstract
A set of extrusion samples of Al±Si±Mg alloys (0.5 wt%Mg and 0.3±0.8 wt%Si) were, respectively, T1- and T4-heat-treated. Differential
scanning calorimetry (DSC) was used to heat the samples to particular temperatures to promote the formation of precipitates for study by
transmission electron microscopy (TEM). It was found that, apart from b 00 , b 0 , and B 0 , there were many precipitates showing rectangular
lattices when viewed along the long axes of the precipitates. It is considered that the residual stresses (or dislocations) in the extrusion after
the T1-treatment facilitated the nucleation and growth of the precipitates during the heating in the DSC. q 2001 Elsevier Science Ltd. All
rights reserved.
Keywords: TEM; Al±Mg±Si; Precipitation; Extrusion; Heat-treatment

1. Introduction Table 1 lists the types of precipitates found so far mostly

6000-series Al±Mg±Si wrought alloys are widely used in
architectural and structural applications because of their
favourable combination of strength, ease of manufacturing
(including extrudability, formability and weldability) and
resistance to stress-corrosion cracking (Polmear, 1995a;
Sheppard, 1999). During production, the extrusions are
commonly `press-quenched' using water sprays and/or air
cooling, depending on the type of the alloy, at the outlet of
extrusion press. Either natural ageing (T1-condition) or arti-
®cial ageing (T5/T6-condition) is then applied to these extru-
sions. In some cases, as-extruded material is given a full
solution treatment, quench and natural age (T4-condition).
For 6000-series alloys, heat treatment is used to promote
the formation of needle-shaped precipitates from the super-
saturated solid solution of Mg and Si in Al to achieve appre-
ciable mechanical properties (Polmear, 1995b; Parson and
Liu, 1988). The type of precipitate that gives rise to the
maximum strength of 6000 alloys in the T6-condition is
designated b 00 , which has been found in electron diffraction
studies to have a body centred monoclinic unit cell,
a ˆ 15.34 A Ê , b ˆ 4.05 A Ê , c ˆ 6.83 AÊ and b ˆ 1068
(Edwards et al., 1994) and an Mg5Si6 stoichiometry (Zand-
bergen et al., 1997). These precipitates are ®ne needles,
,30 nm long, lying parallel to the k001l directions of the
matrix. When the alloy is over-aged, b 00 precipitates are
dissolved and a number of coarser precipitates formed.
* Corresponding author.
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PII: S 0968-432 8(00)00095-0
in over aged materials of these alloys, the nomenclature
used in the literature to refer to the precipitates and that
used for precipitates found in the present work.
It is worth mentioning here that amongst the precipitates
listed in Table 1, Type C precipitates are considered to be
different from B 0 (or Q 0 ) because the former were found in
pure Al±Mg±Si alloys (Matsuda et al., 1996) whilst the
latter were considered to be related to the equilibrium
phase Q (Al5Cu2Mg8Si6) in Al±Cu±Mg±Si alloys (Dumolt
et al., 1984; Suzuki et al., 1979; Chakrabarti et al., 1998).
Types A, B and C precipitates and Si were found in high-Si
alloys (Matsuda et al., 1996; Zhen et al., 1997).
Apart from the microstructural characterisation, thermal
analyses (e.g. DSC) have also been extensively carried out
to unveil the thermal events associated with the precipita-
tion. Previous DSC work on solution-treated 6000-series
alloys showed that the formation of b 00 precipitates produces
a strong exothermic peak at ,2508C and that of b 0 and/or B 0
precipitates shows a peak at ,2908C (Dutta and Allen,
1991; Zhen and Kang, 1998). The peak due to the clustering
of Mg and Si atoms in the early stage of ageing was found at
,808C (Edwards et al., 1994) whereas the peak correspond-
ing to Si precipitates was found at ,3308C (Zhen and Kang,
1998). Increased Si content in the alloy had no pronounced
effect on the precipitation of b 00 and B 0 , but did affect the
formation of Si precipitates (Zhen et al., 1997).
The introduction of mechanical deformation as part of the
heat treatment process in production can signi®cantly
in¯uence the age hardening of 6000-series alloys (Rack
866 J.Y. Yao et al. / Micron 32 (2001) 865±870

Table 1
A variety of precipitates having been found in slightly over-aged 6000-series alloys

Designation Crystal structure Reference Symbol used in this work

b 0 Ê , c ˆ 4.05 A
Hexagonal: a ˆ 7.05 A Ê Jacobs (1972) b0
Close packed hexagonal: a ˆ 4.07 A Ê , c ˆ 4.05 A
Ê Matsuda et al. (1994a)
B 0 or Q 0 Ê , c ˆ 4.04 A
Hexagonal: a ˆ 10.4 A Ê Dumolt et al. (1984); Suzuki et al. (1979); B0
Chakrabarti et al. (1998)
Type A Ê , c ˆ 6.7 A
Hexagonal: a ˆ 4.05 A Ê Matsuda et al. (1996) 4£7
Type B Orthorhombic: a ˆ 6.84 A Ê , b ˆ 7.93 A
Ê , c ˆ 4.05 A
Ê Matsuda et al. (1996) 7£8
Type C Ê , c ˆ 4.05 A
Hexagonal: a ˆ 10.4 A Ê Matsuda et al. (1996) B0
Si Ê
Cubic: a ˆ 5.43 A Zhen et al. (1997) Si

and Krenzer, 1977). This is of considerable interest in
manufacturing processes such as extrusion, forging and roll-
ing, in which the alloy is subjected to extensive deformation
to produce a desirable shape. It has been found, for example,
that cold rolling prior to solution treatment could decrease
the exothermic peak positions of b 00 and Si in DSC (Zhen
and Kang, 1998), whereas cold rolling before ageing could
alter the morphology of precipitates (Matsuda et al., 1994b).
Furthermore, when a solution-treated alloy 6061 was
mechanically deformed (,50%) prior to heating in DSC,
it was found that the peak at 2908C disappeared and, corre-
spondingly in TEM, B 0 precipitates were found to form on
dislocations at the temperatures for b 00 precipitation, that is
,2508C (Edwards et al., 1994). In an in situ TEM study, the
growth of b 0 precipitates was accelerated by the presence of
dislocations (Shewman, 1963).
The industrial practice of a full solution treatment to
achieve speci®c properties requires additional processing
steps and is therefore often avoided whenever possible.
Solution treatment, however, serves metallurgically impor-
tant functions, which include dissolving precipitates
remaining after or formed during extrusion, relieving
`stress' resulting from the combination of deformation and
quenching, and enabling the maximum alloy strength to be
achieved by ageing. The need to further develop our under-
standing of the effects of press-quenching on precipitation
and mechanical properties is thus evident.
The present work is concerned with the in¯uence of heat
treatment (press-quenching vs full solution treatment) and
alloy composition on the precipitation process in extrusions
of a set of experimental alloys. In this work, DSC was used
to heat the sample to selected temperatures to allow the
precipitates to develop to various stages for investigation
by TEM. The samples were produced with an industrial
press and heat-treated to T1- and T4-conditions, respec-
tively, as speci®ed in Section 2. The results from our inves-
tigation showed clearly that, of the two treatments, the T1-
treatment accelerated the precipitation process signi®cantly.
a nominal 0.5 wt%Mg content were selected for study. The
actual compositions of the alloys studied in this paper are
shown in Table 2. The cast billets (f ˆ 127 mm) were
homogenised at 5708C for 2.5 h. For extrusion, the billets
were induction heated to 4508C and extruded to a solid
rectangular section (6 £ 40 mm) using an 880t Cheng Hua
direct extrusion press. The die and container temperatures
were kept at 4358C and 4258C, respectively. The extrudate
speed was ,20 m/min, with water quenching from an exit
temperature of ,5008C.
The practical heat treatment conditions evaluated were:
² T1: water-quenched from press, stretched 0.5%, and
naturally aged for more than a week;
² T4: as for T1, then solution-treated for 1 h at 5208C,
followed by cold water quench and naturally aged for
more than a week.
For the TEM investigation, disc shaped samples
(,0.5 mm thick) were prepared from the extrusion and
then heat-treated in DSC. They were heated at 108C/min
to selected temperatures in a Perkin Elmer DSC7 instrument
and then immediately removed from the testing pan. Fig. 1
contains DSC thermograms typical of the T1- and T4-trea-
ted alloys. The temperatures at which the samples were
removed from DSC are also indicated. (Note that the DSC
curves for each alloy and heat treatment in Fig. 1 have been
offset for presentation clarity.) T1-treated alloys had one
broad exothermic peak between 200 and 3508C. T4-treated
alloys had, however, one exothermic peak for alloy 1 and
two exothermic peaks for alloys 4 and 5 in between 200 and
3508C. In other words, with increasing Si content, the ®rst
peak in T4-treated alloys shifted to lower temperatures and
was resolved into two peaks. There was no clear peak shift
for the T1-treated alloys with increasing Si content.
Table 2
Compositions (wt%) of the Al±Mg±Si alloys studied

Alloy no. Si Mg Fe Cu Al

2. Experimental 1 0.27 0.49 0.10 , 0.01 Balance

4 0.62 0.48 0.12 , 0.01 Balance
5 0.77 0.47 0.10 , 0.01 Balance
Alloys with a wide range of Si content (0.3±0.8 wt%) and
 J.Y. Yao et al. / Micron 32 (2001) 865±870
Fig. 1. DSC thermograms of T1-and T4-treated extrusion samples of alloys
1, 4 and 5 with nominal 0.5 wt%Mg and varying Si contents. Samples for
TEM investigation were heated to the temperatures as indicated by the open
circles on the curves.
The TEM lattice imaging investigation was performed
with a JEOL 4010 instrument operating at 400 keV, whereas
the diffraction contrast investigation was conducted with a
JOEL 2010 instrument operating at 200 keV. The thin foil
specimens were prepared from the samples treated in DSC
by electro-chemical polishing for the diffraction contrast
investigation. For lattice imaging the specimens were
further thinned by ion beam thinning while the specimen
was cooled with liquid nitrogen. The precipitates in each
sample were identi®ed by examining the lattice periodicity
on the TEM images, which were taken from the transversal
cross-section of the precipitates.
3. Results
For the low-Si alloy (alloy 1), only b 0 precipitates were
found after heating to 300 and 3408C for the T1- and T4-
samples, respectively. For the high-Si alloys (alloys 4 and
5), different types of precipitates were observed. Typical
lattice imaging micrographs of the different precipitates
are shown in Fig. 2.
The number count of precipitates examined by TEM are
summarised in Table 3. The approximate percentages of
each precipitate type (B 0 , b 0 , 4 £ 7 and 7 £ 8) are also
shown. Complex precipitates consisted of more than one
type of precipitate.
4. Discussion
4.1. Low-Si alloy
When the specimens of alloy 1 were heated just over the
exothermal peak in DSC (viz, ,3008C for T1 and 3408C for
T4 as indicated in Fig. 1), only b 0 precipitates were found by
867
the TEM (Table 3). This observation suggests that the preci-
pitation process in this alloy for T1- and T4-treatments may
be similar, with T1-precipitation being accelerated. The
peak was shifted about 408C towards the low temperature
end (i.e. the peak was at ,2508C for T1- and T4-peak at
,2908C).
The microstructural differences created by the T1- and
T4-heat treatments are expected to be the density of dislo-
cations due to stretching for the T1-samples, and the levels
of Mg and Si in the matrix available for precipitation (if the
extrusion process has not fully solutionised the Mg and Si).
Fig. 3 shows a TEM bright ®eld image taken from a T1-
treated alloy 1 specimen which was DSC heated to 2208C,
just before the start of the exothermic peak at ,2508C. At
this early state of precipitation, ®ne precipitates began to
form in the vicinity of dislocations (as arrowed), whereas no
precipitates were observed in dislocation-free regions.
Though the type of precipitate has not been successfully
identi®ed, the heterogeneous nucleation of precipitates at
the dislocations was evident. The presence of dislocations
in the alloy from the T1-treatment has provided a substantial
number of sites for the heterogeneous nucleation of preci-
pitates, which is more favourable than homogeneous
nucleation. A number of effects can further accelerate the
precipitation from dislocations, including the accelerated
diffusion of solute atoms along dislocations (Shewman,
1963) and the additional supply of vacancies to precipitates
by dislocation climb (Beaven et al., 1982). This dislocation-
assisted precipitation would have enabled the nucleation
and development of precipitates to occur at temperatures
lower than those for homogeneous nucleation.
Further work is needed to unveil the precipitation process
associated with various positions of the exothermal peak in
order to understand how the dislocation assisted precipita-
tion mechanism has reduced the temperature for the highest
rate of precipitation, which is presumably due to the preci-
pitation of b 00 rather than b 0 .
4.2. High-Si alloys
For high-Si alloys (i.e. alloys 4 and 5), a number of differ-
ent types of precipitates were observed. After heating in
DSC to 2908C, similar proportions of the different precipi-
tates were observed for the T1- and T4-treatments. For alloy
4, most precipitates were found to be B 0 or 7 £ 8 types, with
fewer b 0 and 4 £ 7 precipitates. For alloy 5, similar propor-
tions of B 0 , 4 £ 7 and 7 £ 8 precipitates were observed.
However, after heating to 3208C in DSC, differences
between the T1- and T4-treated samples are evident.
Alloy 4 T4 shows further development of b 0 indicated by
the percentage increase of b 0 from ,20% at 2908C to ,70%
at 3208C, and a reduction in the B 0 and 7 £ 8 precipitates is
observed. This is in contrast to the precipitates formed in the
T1-treated sample of alloy 4, where B 0 precipitates were
dominant, ,40% at 2908C increasing to ,90% at 3208C.
It appears that the T1-treatment has facilitated the
868 J.Y. Yao et al. / Micron 32 (2001) 865±870

Fig. 2. Typical [001]Al lattice imaging of (a) B 0 in alloy 5 (T1) DSC±2908C, (b) b 0 in alloy 4 (T4) DSC-3208C, (c) b 00 in alloy 5 (T4) DSC-2908C, (d) 7 £ 8,
alloy 4 (T4) DSC-2908C, (e) 4 £ 7, alloy 5 (T1) DSC-2908C, and (f) 4 £ 7-b 0 complex in alloy 4 (T4) DSC-3208C.

development of B 0 precipitates and T4 favours b 0 precipita-
tion during overageing for this alloy composition.
In order to estimate the signi®cance of the apparent
trends, as described above, further investigation is needed.
However, it seems to be impractical to use the high resolu-
tion TEM method (which is used in this work) to better
quantify the proportion of each type of precipitate formed
by increasing the number of precipitates to examine. The
presence of local microstructural inhomogeneity (e.g. the
location and density of dislocations and dispersiods) may
affect the local precipitation kinetics by offering nucleation
sites for precipitation and sinks for vacancies. This could
seriously affect the results of TEM lattice imaging as this
method examines precipitates on a scale smaller than, or
similar to, the structural inhomogeneity.
Nevertheless, the TEM results of the high-Si alloys high-
lighted the complexity of the precipitation process which
gave rise to the peaks in the DSC. The presence of the
 J.Y. Yao et al. / Micron 32 (2001) 865±870 869

Fig. 2. (continued)

second DSC peak of the T4-treated alloys does not seem to
be due to the formation of one type of precipitate which,
somehow, has not formed in the corresponding T1-treated
alloys. After all, the essential microstructural difference
between the T1- and T4-treated alloys is the density of
dislocations. The T4-treated alloys have lower dislocation
density than the T1-treated alloys, but they are far from
dislocation free. Thus one needs to know not only the
type of precipitate, but also the locations where they form
in order to understand the associated precipitation process
which gives rise to the second DSC peak for T4-treated
high-Si alloys.
5. Summary
Precipitation in Al±Mg±Si alloy extrusions has been
investigated by TEM, for alloys with nominal 0.5 wt%Mg
and a range of alloy Si contents, and for two heat treatment
processes (press-quenched and stretched T1-condition and
solution-treated T4-condition). It has been found that the
T1-treatment accelerated the precipitation process in the
low-Si content alloy, and b 0 was observed in the slightly
over-aged conditions. This acceleration diminished for
high-Si alloys and the ageing favoured initial formation of
B 0 , b 0 , 4 £ 7 and 7 £ 8 precipitates, which had already
nucleated when the alloys were heated to 2908C in DSC.
Further development of b 0 for T4-condition occurred in the
high-Si alloy heated to 3208C.
Acknowledgements
This work was performed with the support of the CRC for
Cast Metals Manufacturing (CAST) and Comalco Alumi-
nium Ltd. CAST was established under the Australian
Government's Cooperative Research Centres Scheme.

Table 3
The number of precipitates observed by TEM in specimens heat-treated in DSC

Alloy (temper) Temp. (8C) b 00 B0 b0 4£7 7£8 Complex

1 (T1) 300 17 (100%)

1 (T4) 340 7 (100%)
4 (T1) 290 2 22 (40%) 4 (10%) 10 (20%) 16 (30%) 9
320 12 (90%) 1 (10%) 1
4 (T4) 290 6 (40%) 3 (20%) 2 (10%) 4 (30%) 1
320 11 (70%) 4 (30%) 1 3
5 (T1) 290 6 (20%) 1 7 (30%) 14 (50%) 2
5 (T4) 290 1 6 (35%) 5 (30%) 6 (35%) 2
870 J.Y. Yao et al. / Micron 32 (2001) 865±870
Fig. 3. TEM bright ®eld image of a specimen of T1-treated alloy 1, which
was heated to 2208C in DSC, showing the heterogeneous nucleation of
precipitates at dislocations.
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