The Effect of Homogenization Practice On The Microstructure of AA6063 Billets

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The effect of homogenization practice on the microstructure of AA6063 billets

Article  in  Journal of Materials Processing Technology · May 2004


DOI: 10.1016/j.jmatprotec.2004.01.056

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Journal of Materials Processing Technology 148 (2004) 250–258

The effect of homogenization practice on the microstructure


of AA6063 billets
Yücel Birol∗
Materials and Chemical Technologies Research Institute, Marmara Research Center, TUBITAK, Gebze, Kocaeli, Turkey
Received 20 March 2003; accepted 16 January 2004

Abstract

It is well established that homogenized billets extrude easier and faster and give better surface finish and higher tensile properties than
as-cast billets. Hence, the production of Al–Mg–Si extrusions from DC-cast billets almost always starts with a homogenization cycle
which typically consists of a soaking treatment followed by cooling at a predetermined rate. While soaking is performed to produce a
homogeneous solid solution and to transform the ␤-AlFeSi particles to the more acceptable ␣ variety, the motivation behind controlled
cooling is heterogenization. The cooling cycle has to be designed to reprecipitate as much Mg2 Si as possible, in a form and size easily
redissolvable during subsequent processing for high extrudability and surface quality. The effect of various soaking and cooling cycles on
the formation and transformation of insoluble and soluble constituents was investigated in order to identify the optimum homogenization
practice for a semicontinuous DC-cast AA6063 billet. A homogenization practice with a 6 h soak at 580 ◦ C followed by step-cooling at
250–300 ◦ C was found to be optimum. Step-cooling gave a more complete depletion of the aluminum solid solution, i.e. lower flow stress,
without forming coarse and stable Mg2 Si particles which are very difficult to solutionize during reheating and thus survive the extrusion
process impairing both surface quality and mechanical properties.
© 2004 Elsevier B.V. All rights reserved.

Keywords: Homogenization; Extrusion; AA6063; Microstructure

1. Introduction An industrial homogenization practice typically consists


of a soaking treatment which is followed by cooling at a
It is well established that homogenized billets extrude predetermined rate [3]. Several processes take place during
easier and faster and give better surface finish and higher soaking [4,5]. The interdendritic network of the plate-like
tensile properties than as-cast billets [1]. However, there ␤-AlFeSi intermetallics are replaced by the more rounded
are limits to how much a homogenization treatment can discrete ␣-AlFeSi particles. The ␤ → ␣ transformation is
improve the performance of the billet on the press. There important as the ␤-AlFeSi particles are often held respon-
are several features that must be imparted to the billet be- sible for a number of surface defects, limiting extrudability
fore homogenization, in the cast house. The billet chemistry [5–9]. The Mg2 Si particles and coarse eutectics are also so-
has to be optimized in accordance with the needs and ex- lutionized in a soaked billet [5,10,11] while the coring inher-
pectations of the extruder. A cast billet should also have ited from the as-cast microstructure is leveled out in favor of
fine grain and cell structure uniformly distributed over its a more homogeneous distribution of the solute Mg and Si.
cross-section, no coarse script intermetallics, minimum sur- Unfortunately, a fully solutionized billet as obtained at
face segregation and shell zone and an acceptable surface the end of soaking, is difficult to extrude. So, in contrast
finish [2]. When properly homogenized, such a billet will to soaking which is undertaken to achieve homogenization,
give high throughput rates, low breakout pressures, desired the motivation behind controlled cooling is heterogenization
shape within dimensional tolerances, uniform surface fin- [12]. Slow cooling tends to produce coarse Mg2 Si particles
ish free from streaking, pick-up, die-lines as well as high while rapid cooling traps the Mg and Si in solution with
tensile properties. little or no Mg2 Si precipitation [13–15]. Coarse ␤-Mg2 Si
particles are difficult to solutionize at common preheating
∗ Present address: The Scientific and Technical Research Council of temperatures, resist solutionizing at high heating rates and
Turkey, Marmara Research Centre, PO Box 21, 41470 Gebze, Kocaeli, may even survive the extrusion process. Such particles lead
Turkey. to incipient melting and surface tearing during extrusion,

0924-0136/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2004.01.056
Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258 251

giving poor surface quality and are also responsible for poor Table 1
tensile properties. Mg and Si in solution, on the other hand, The chemical composition of the AA6063 alloy used in the present
investigation (wt.%)
have an adverse effect on the flow stress of the alloy and
thus increase its resistance to deformation. So, the cooling Si 0.429
cycle has to be designed to reprecipitate as much Mg2 Si Mg 0.446
Fe 0.218
as possible, in a form and size easily redissolvable during Mn 0.004
subsequent processing. Cu 0.003
The present work was undertaken to investigate the effect Ti 0.017
of various soaking and cooling cycles on the formation and Al 98.80
transformation of insoluble and soluble constituents and to Siex 0.097
Mg2 Si 0.704
identify the optimum homogenization practice for a semi-
continuous DC-cast AA6063 billet.
35 mm wide and 10 mm thick, were sectioned from a
transverse slice of the billet, at least 10 mm away from
2. Experimental the surface, in each case, to avoid possible microstruc-
tural and compositional variations from one sample to the
The AA6063 alloy used in the present investigation was other.
cast industrially with a vertical DC caster in the form of 6 m Soaking experiments were performed in the tempera-
long billets with a diameter of 152 mm. Its chemical compo- ture range 540–580 ◦ C with a 2–6 h soak (Fig. 1a). One of
sition is given in Table 1. Due to the very low Mn content, the two sets of soaked samples were air-quenched as the
the present alloy relied solely on the soaking practice for the focus was on the evolution of the insoluble constituents.
␤ → ␣ transformation. The Mg2 Si content of the present The second set of samples were cooled to approximately
alloy suggests that it was produced for high extrudability 200 ◦ C at a rate of 200 ◦ C/h to facilitate precipitation of
rather than high strength. the Mg2 Si phase in order to evaluate the precipitation pat-
Homogenization trials were performed first by changing tern and judge the homogenization of the solid solution
the soaking parameters but employing a constant cool- matrix. Soaked samples were prepared with standard met-
ing rate and then by changing the cooling practice but allographic techniques: ground with SiC paper, polished
keeping the soak time and temperature constant (Fig. 1). with 3 ␮m diamond paste and finished with colloidal silica.
Samples for both soaking and cooling trials, 65 mm long, They were examined after etching with a 0.5% HF solu-

Fig. 1. Soaking and cooling cycles employed in the present work.


252 Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258

tion using a Olympus BX51M model optical microscope.


The XRD patterns were recorded with a Shimadzu XRD
6000 Diffractometer equipped with Cu K␣ radiation. The
diffractometer was operated at very low scanning rates to
increase the counting frequency. A Voyager 2110 model
energy dispersive X-ray analyzer (EDS) was also used for
further identification of the intermetallic phases. Soaked
samples were investigated for the extent of ␤-AlFeSi →
␣-AlFeSi transformation, solutionizing of the coarse Mg2 Si
particles and for the homogenization of the solid solution
matrix.
The effect of cooling practice on the precipitation of
Mg2 Si particles was investigated by employing two differ-
ent types of cooling cycles following a 6 h soak at 580 ◦ C
(Fig. 1b). The first of these involved continuous cooling
at rates ranging from air cooling to 12 ◦ C/h. For the size
of the specimens used in the present study, air cooling
corresponded to a cooling rate of 2000 ◦ C/h. Temperatures
were recorded directly from the samples as a function of
time and measures were taken to establish a constant cool-
ing rate down to 200 ◦ C at which point all samples were
air-quenched. The second set of cooling experiments in-
volved a 2 h isothermal step at various temperatures between
450 and 200 ◦ C. Samples soaked at 580 ◦ C for 6 h were
air-quenched before and after the 2 h isothermal step. These
samples were investigated for the extent of Mg2 Si precip-
itation and for the size of the Mg2 Si particles. They were
examined after etching with a 0.5% HF solution using an
Olympus BX51M model optical microscope. Samples were
slightly overetched to facilitate direct observation of the fine
Mg2 Si particles with the light microscope. Dark-field imag-
ing was also employed to improve resolution. The electrical
conductivity of the samples was measured with a Sigma
Test Unit for the evaluation of the extent of the precipitation
activities.
Differential scanning calorimetry (DSC) was employed
to investigate how the homogenized samples cooled at dif-
ferent rates and with an isothermal step at different tem-
peratures would respond to a reheating treatment. A Poly-
mer Laboratories DSC unit was used and the samples were
heated under flowing argon at a rate of 20 ◦ C/min until before
melting.

3. Results and discussion


Fig. 2. (a) Microstructure of the as-cast billet, (b) the shell zone at the
surface and (c) macrostructure showing the grains and the segregation
3.1. As-cast billet pattern.

The microstructure of the as-cast billet consisted of


primary dendrites of aluminum rich solid solution with a
well-defined interdendritic network of ␤-AlFeSi platelets generally free of coarse intermetallics (Fig. 2b), while the
(Fig. 2a). There was hardly any evidence for the Mg2 Si average grain size was estimated to be 150 ␮m (Fig. 2c).
phase, owing to a high enough cooling rate during solidifi- Both the cell size and the grain size were uniform across
cation which apparently retained the Si remaining from the the cross-section of the billet. It was thus concluded, from
insoluble constituents and Mg in solid solution. The shell the metallographic analysis that the as-cast billet was of
zone in the cast billet was less than 100 ␮m deep and was adequate quality.
Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258 253

Fig. 3. The microstructural features of samples soaked between 540 and 580 ◦ C for 2–6 h and subsequently air-quenched.

3.2. Soaking experiments platelets broke up into relatively small discrete particles after
soaking at this temperature. The latter were responsible for
Fig. 3 illustrates the microstructures of those samples that the new reflections in the XRD spectrum that were readily
were soaked between 540 and 580 ◦ C for 2–6 h and subse- indexed by the hexagonal ␣-AlFeSi phase. The ␤-AlFeSi
quently air-cooled. Soaking at 540 ◦ C for 2 h seemed to have particles that have survived soaking implied that the ␤ →
produced little change in the type and distribution of AlFeSi ␣ transformation was still not complete at 560 ◦ C. Further
phases. The majority of the interdendritic particles were still evidence for the hexagonal ␣ phase becoming the major
plate-like and were identified by XRD to be of the ␤-AlFeSi phase was provided by the EDS work that gave a Fe/Si ratio
variety suggesting that the ␤ → ␣ transformation at this between 1.5 and 2 for the majority of the particles analyzed.
temperature was very sluggish. ␤-AlFeSi was still the ma- The change in the microstructural features outlined above
jor phase in those samples soaked at 540 ◦ C for 4 and 6 h in has become more prominent after soaking at 580 ◦ C. The
spite of an increasing number of particles that were identi- ␤-AlFeSi phase was clearly the minor phase only after 2 h at
fied by EDS to be of the hexagonal ␣-AlFeSi type (Table 2). this temperature (Table 2). The interdendritic platelets were
Both structural and morphological features of the cast replaced almost entirely by discrete round particles, giving
billet have changed considerably starting at 560 ◦ C. The ␤ a “necklace” type configuration. The ␤-AlFeSi phase has

Table 2
The insoluble constituents in soaked billets
Temperature (◦ C) Time (h)

2 4 6

540 ␤-AlFeSi, ␣-AlFeSi ␤-AlFeSi, ␣-AlFeSi ␤-AlFeSi, ␣-AlFeSi


560 ␣-AlFeSi (␤-AlFeSi) ␣-AlFeSi (␤-AlFeSi) ␣-AlFeSi (␤-AlFeSi)
580 ␣-AlFeSi (␤-AlFeSi) ␣-AlFeSi (␤-AlFeSi) ␣-AlFeSi
The major constituent is underlined; the minor ones are put into parentheses. The constituents are listed in the order of their volume fractions.
254 Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258

Fig. 4. The distribution of Mg2 Si precipitates in a sample soaked at: (a) 540 ◦ C for 2 h and (b) 560 ◦ C for 4 h subsequently cooled to 200 ◦ C at 200 ◦ C/h.

completely transformed after 6 h soaking at 580 ◦ C while nied by a remarkable change in the microstructural features
nearly equal number of hexagonal and cubic ␣-AlFeSi par- of these samples. The population of the Mg2 Si precipitates
ticles were encountered in EDS analysis. was reduced drastically as the very fine and dense disper-
The microstructures of the two of the samples which were sion was replaced by relatively coarse, stable precipitates
given a 6 h soak at 580 ◦ C and subsequently cooled at a rate when the cooling rate dropped below 100 ◦ C/h (Fig. 5). The
of 200 ◦ C/h to allow for Mg2 Si precipitation are shown in increasing conductivity values in this range suggested that
Fig. 4. The distribution of Mg2 Si particles in samples soaked the depletion of the solid solution matrix was still underway
at 540 ◦ C revealed a heterogeneous character inherited from (Table 3). The coarsening of the Mg2 Si precipitates contin-
the as-cast microstructure suggesting that the microsegrega- ued further with decreasing cooling rate as evidenced by the
tion was yet not removed. The sample soaked at 560 ◦ C for increase in the population of coarse Mg2 Si particles at the
4 h, on the other hand, showed a more uniform distribution of expense of finer ones in the sample cooled very slowly at
Mg2 Si particles. It is thus claimed that a soaking treatment 12 ◦ C/h.
of at least 4 h at 560 ◦ C is required to eliminate segregation Fig. 6 shows the DSC scans of the samples soaked at
and to even out the Mg and Si distribution in the matrix. 580 ◦ C for 6 h and cooled very fast to very slowly, in the
range 2000–12 ◦ C/h. Results of the optical microscopy, elec-
trical conductivity measurements and the XRD work were
3.3. Cooling experiments paralleled by the DSC analysis of these samples. The ther-
mograms of the samples cooled at 400 ◦ C/h and faster re-
3.3.1. Continuous cooling vealed a total of four well-defined peaks until 600 ◦ C (Fig. 6).
The post-homogenization cooling rate appeared to have The first three of these peaks are exothermic and are thus
a profound effect on the precipitation and dispersion char- associated with precipitation activities while the last one
acteristics of the Mg2 Si phase, as expected. The samples is endothermic and indicates a dissolution reaction. The
soaked at 580 ◦ C for 6 h and subsequently air-cooled (at first exothermic peak is rather small and occurs at approxi-
a rate of 2000 ◦ C/h) hardly revealed any Mg2 Si precipi- mately 140 ◦ C. It is claimed to be associated with the forma-
tates (Fig. 5). It is thus concluded that the Mg2 Si particles tion of Mg–Si clusters. The precipitation of the metastable
were fully solutionized after soaking at 580 ◦ C and that the ␤ /␤ -Mg2 Si and the stable ␤-Mg2 Si particles were respon-
free Si and the Mg were both retained in solution during sible for the second and third exothermic peaks, respectively.
air-cooling. The population of very fine Mg2 Si particles The endothermic peak which is estimated to start at 450 ◦ C,
inside the dendrites increased with decreasing cooling rates
and finally, the samples cooled at 100 ◦ C/h were crowded Table 3
with such particles. The precipitation of Mg2 Si particles was Electrical conductivity values of the samples soaked at 580 ◦ C for 6 h and
apparently not random and those sites with relatively higher subsequently cooled at different rates
energy were decorated first upon precipitation. The increas- Cooling rate (◦ C/h) Electrical conductivity (m/ mm2 )
ing precipitation activity with decreasing cooling rates was
2000 28.6
reflected also by increasing conductivity values (Table 3). 800 28.7
Mg2 Si precipitates were either too few and/or too fine to 400 29.0
give a detectable signal in the XRD spectrum, in all sam- 200 29.6
ples cooled at 100 ◦ C/h or faster. Reflections of the cubic 100 30.1
30 31.0
equilibrium Mg2 Si phase were noted, however, after cooling
12 32.0
at 30 ◦ C. This change in the XRD response was accompa-
Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258 255

Fig. 5. Dark-field optical micrographs showing the distribution of Mg2 Si precipitates in samples soaked at 580 ◦ C for 6 h and subsequently cooled to
200 ◦ C at: (a) 2000 ◦ C/h, (b) 800 ◦ C/h, (c) 400 ◦ C/h, (d) 200 ◦ C/h, (e) 100 ◦ C/h, (f) 30 ◦ C/h and (g) 12 ◦ C/h.

on the other hand, represents the solutionizing of the equi- slow cooling at 12 ◦ C/h. There was hardly any Mg and Si
librium ␤-Mg2 Si phase, i.e. the solvus temperature. left in solution to precipitate during reheating when the bil-
The intensity of the exothermic peaks correlates very well let was cooled from the soaking temperature very slowly.
with the homogenization cooling rate. The higher precipita- The broad exothermic effect observed in the samples cooled
tion capacity of those samples cooled at 2000 and 800 ◦ C/h, slowly at 30 and 12 ◦ C/h are claimed to be due to further
is demonstrated by their relatively larger exothermic peaks. coarsening of the stable Mg2 Si precipitates.
The intensity of these peaks is reduced with decreasing cool- The temperature range of the dissolution peak is of great
ing rate suggesting that increasing amounts of Mg2 Si precip- technological interest as it signals the potential problems
itation has already taken place during post-homogenization that are often encountered with respect to surface quality
cooling. Finally, the exothermic peaks were very weak at and hardening capacity. The solutionizing of the Mg2 Si pre-
30 ◦ C/h and were completely missing in the case of very cipitates was over at approximately 500 ◦ C, well below the
256 Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258

press exit temperatures commonly encountered in industrial


practice in all samples cooled from the soaking temperature
faster than 100 ◦ C/h. A small additional endothermic effect
appeared during reheating of the sample cooled at 100 ◦ C/h,
suggesting that coarse cubic ␤-Mg2 Si precipitates, in addi-
tion to the very fine ones, have formed at this cooling rate.
The endothermic peaks were displaced to still higher tem-
peratures (by as much as 50 ◦ C) in the samples cooled at
30 and 12 ◦ C/h. While the fine, metastable Mg2 Si particles
which form at high cooling rates respond to preheating read-
ily, coarse ␤-Mg2 Si particles are apparently stable at high
temperatures and are thus more difficult to dissolve during
reheating as evidenced by the displacement of the dissolu-
tion peak to higher temperatures in the DSC scans of the
samples cooled at or slower than 30 ◦ C/h.
It is thus concluded that post-homogenization cooling
faster than 100 ◦ C/h should be employed for the present
Fig. 6. DSC scans of the samples soaked at 580 ◦ C for 6 h and cooled at alloy in order to avoid the formation of coarse Mg2 Si
various rates, in the range 12–2000 ◦ C/h. The heating rate was 20 ◦ C/min. precipitates which would be difficult to solutionize during

Fig. 7. Dark-field optical micrographs showing the distribution of Mg2 Si precipitates in samples soaked at 580 ◦ C for 6 h and step-cooled at: (a) 450 ◦ C,
(b) 400 ◦ C, (c) 350 ◦ C, (d) 300 ◦ C, (e) 250 ◦ C and (f) 200 ◦ C.
Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258 257

reheating and extrusion. A cooling rate below 200 ◦ C/h is Table 4


desired, on the other hand, to achieve an effective depletion Electrical conductivity values of the samples soaked at 580 ◦ C for 6 h and
subsequently cooled at different isothermal hold temperatures
of the solid solution matrix for a low flow stress and low
resistance to extrusion deformation. Isothermal-step temperature (◦ C) Electrical conductivity
(m/ mm2 )
3.3.2. Step-cooling 450 28.8
400 30.1
The temperature of the isothermal step inserted in the
350 31.3
cooling cycle influenced Mg2 Si precipitation just as much 300 31.6
as the cooling rate did in continuous cooling cycles. De- 250 31.6
creasing the isothermal-step temperature seemed to produce 200 29.2
an effect similar to that of decreasing the cooling rate. The
samples soaked at 580 ◦ C for 6 h and air-quenched before
and after a 2 h isothermal hold at 450 ◦ C did not reveal any isothermal-step temperatures was reflected by increasing
Mg2 Si precipitates (Fig. 7). This was confirmed also by the conductivity values until 300 ◦ C. The extent of the precipi-
electrical conductivity of this sample which was nearly equal tation was more or less the same in the sample step-cooled
to that of the soaked and quenched (supersaturated) sample. at 250 ◦ C as inferred from a very similar electrical conduc-
Hence, the solvus temperature is claimed to be slightly below tivity value. Lack of precipitation at 200 ◦ C is evidenced
450 ◦ C for the present alloy and Mg2 Si, if any, were solu- also by the sudden drop in the electrical conductivity of this
tionized rather than precipitated after 2 h at this temperature. sample.
Some precipitation activity was first noted after step-cooling Fig. 8 shows the DSC scans of the samples soaked at
at 400 ◦ C with an accompanying increase in electrical con- 580 ◦ C for 6 h and step-cooled at various temperatures
ductivity. The precipitation at this high temperature has pro- between 200 and 450 ◦ C. Results of optical microscopy,
duced a very coarse dispersion of the stable cubic ␤-Mg2 Si electrical conductivity measurements and XRD work were
particles. The population of Mg2 Si particles increased but paralleled by the DSC analysis of the step-cooled samples.
their size decreased with decreasing isothermal-step temper- The reheating thermogram of the sample step-cooled at
atures. Finally, the sample step-cooled at 250 ◦ C revealed a 200 ◦ C reveal all three exothermic peaks until 600 ◦ C in
very fine dispersion of Mg2 Si particles. The majority of these the addition to the endothermic peak as this temperature
particles were of the metastable ␤ -Mg2 Si variety as evi- was too low to allow any precipitation within 2 h. The two
denced by the lack of their exothermic effect in the calorime- low-temperature exothermic peaks were completely missing
try scan obtained during reheating. The sample step-cooled and the exothermic effect produced by the precipitation of
at 200 ◦ C, on the other hand, were free from any Mg2 Si par- the equilibrium ␤-Mg2 Si phase was very much weakened in
ticles indicating that no precipitation has taken place at this that sample cooled with a 2 h isothermal hold at 250 ◦ C. It
temperature. is thus concluded that much of the available Mg and Si had
Electrical conductivity measurements were in good already precipitated in the form of ␤ /␤ -Mg2 Si particles
agreement with the microstructural observations (Table 4). during the 2 h isothermal hold at this temperature and little
The increasing overall precipitation activity with decreasing Mg and Si were available to precipitate during reheating.

Fig. 8. DSC scans of the samples soaked at 580 ◦ C for 6 h and step-cooled at temperatures between 450 ◦ C and 200 ◦ C. The heating rate was 20 ◦ C/min.
258 Y. Birol / Journal of Materials Processing Technology 148 (2004) 250–258

The thermogram of the sample step-cooled at 300 ◦ C was particles which were readily solutionized during reheating.
almost identical, as one would expect in view of the met- Step-cooling under the conditions described above appears
allographic work and electrical conductivity measurements. to be a better practice than continuous cooling at a rate
A broad exothermic effect was noted during reheating of between 100 and 200 ◦ C/h for optimum billet performance.
the sample step-cooled at 350 ◦ C, as typically observed The former gives a more complete depletion of the alu-
when coarsening processes are active. Exothermic peaks for minum solid solution, i.e. lower flow stresses, avoiding the
the precipitation of both metastable ␤ /␤ -Mg2 Si and stable formation of coarse and stable Mg2 Si particles which are
␤-Mg2 Si particles appeared during reheating of the sample very difficult to solutionize during reheating and thus sur-
step-cooled at 400 ◦ C. The higher solute levels of Mg and vive the extrusion process impairing both surface quality
Si in the sample held at this temperature is responsible for and mechanical properties.
the restoration of the precipitation capacity. A major differ-
ence produced by the isothermal hold at 400 ◦ C is the shift
of the dissolution peak to higher temperatures suggesting Acknowledgements
that the Mg2 Si particles formed during the isothermal hold
and coarsened further during reheating are very difficult to It is a pleasure to thank Miss Selda Üçüncüoǧlu and Mr.
solutionize and are potentially harmful both to the surface Fahri Alageyik for their help in the metallographic work,
quality and mechanical properties. Mr. Osman Çakir for performing the heat treatments, Mrs.
Of the several isothermal-step temperatures tested in Feriha Birol of ARÇELİK for running the DSC tests.
step-cooling experiments, 250 and 300 ◦ C appeared to yield
the best results as they have maximized the precipitation
of Mg2 Si without shifting the dissolution peak to higher References
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Step-cooling at 250–300 ◦ C for 2 h was found to give Extrusion Technology Seminar, vol. 1, Aluminum Association, Wash-
extensive precipitation of the fine, metastable ␤ -Mg2 Si ington, DC, 1996, p. 529.

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