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The Effect of Homogenization Practice On The Microstructure of AA6063 Billets
The Effect of Homogenization Practice On The Microstructure of AA6063 Billets
The Effect of Homogenization Practice On The Microstructure of AA6063 Billets
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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.
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. 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
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
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
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
temperatures.
[1] E.C. Beatty, in: Proceedings of the First International Aluminum
Extrusion Technology Seminar, Paper no. 10, Aluminum Association,
4. Conclusions Washington, DC, 1969.
[2] A.J. Bryant, G.E. Macey, R.A.P. Fielding, Light Met. Age (2002) 6.
[3] Y. Birol, G. Kara, S. Üçüncüoǧlu, M. Usta, in: Z. Jin, A. Beaudoin,
Soaking at 540 ◦ C falls far too short of expectations T.A. Bieler, B. Radhakrishnan (Eds.), Hot Deformation of Aluminum
as it fails to remove microsegregation and to achieve the Alloys III, TMS, 2003, p. 463.
-AlFeSi → ␣-AlFeSi transformation both of which are [4] S.R. Claves, D.L. Elias, W.Z. Misiolek, Materials Science Forum,
vols. 396–402, Trans Tech Publications, Switzerland, 2002, p. 667.
desirable to improve the surface quality and extrudability
[5] S. Zajac, et al., Mater. Sci. Technol. 10 (1994) 323.
of the material. The interdendritic network of the -AlFeSi [6] E.C. Beatty, in: Proceedings of the Second International Aluminum
platelets is replaced by a dispersion of equiaxed, discrete Extrusion Technology Seminar, vol. 1, pp. 225–228.
␣-AlFeSi particles and a homogeneous Al(Mg,Si) solid [7] J. Langerweger, in: Proceedings of the Conference on Aluminium
solution is obtained starting at 560 ◦ C. It takes a 6 h soak Technology, London, March 1986, p. 216.
at 580 ◦ C to fully transform the -AlFeSi phase to the [8] K. Karhausen, A.L. Dons, T. Aukrust, Mater. Sci. Forum 217–222
(1996) 403.
␣-AlFeSi phase in the present alloy with a very low Mn [9] T. Oka, M. Yanagawa, M. Hirano, in: Proceedings of the Sixth In-
level. ternational Aluminum Extrusion Technology Seminar, vol. 1, Alu-
The extent of precipitation increased with decreasing minum Association, Washington, DC, 1996, p. 157.
post-homogenization cooling rates. However, cooling rates [10] N.C.W. Kuijpers, W.H. Kool, S. van der Zwaag, Materials Science
below 100 ◦ C/h produced coarse -Mg2 Si particles that Forum, vols. 396–402, Trans Tech Publications, Switzerland, 2002,
p. 675.
were shown by DSC to be difficult to solutionize during [11] H. Tanihata, et al., J. Mater. Sci. 34 (1999) 1205–1210.
reheating. A cooling rate below 200 ◦ C/h is desired, on the [12] S. Zajac, B. Bengtsson, C. Jonsson, Materials Science Forum, vols.
other hand, to achieve an effective depletion of the solid 396–402, Trans Tech Publications, Switzerland, 2002, p. 399.
solution matrix for a low flow stress and low resistance to [13] E.B. Bjornbakk, et al., Materials Science Forum, vols. 396–402,
Trans Tech Publications, Switzerland, 2002, p. 405.
extrusion deformation. It is thus concluded that a cooling
[14] O. Reiso, et al., in: Proceedings of the Sixth International Aluminum
rate between 200 and 100 ◦ C/h is optimum for the present Extrusion Technology Seminar, vol. 1, Aluminum Association, Wash-
alloy for high extrudability and surface quality should ington, DC, 1996, p. 1.
continuous cooling be employed after soaking. [15] N. Dahl, et al., in: Proceedings of the Sixth International Aluminum
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.