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Met. Mater. Int., Vol. 20, No. 4 (2014), pp.

727~732
doi: 10.1007/s12540-014-4018-x

Effect of Cr and Zr on the Grain Structure of Extruded EN AW 6082 Alloy

Yucel Birol1,2,*

1
Marmara Research Center, Materials Institute, TUBITAK, Kocaeli, Turkey
2
Dokuz Eylul University, Dept. of Metallurgical and Materials Engineering,
Faculty of Engineering, Izmir, Turkey
(received date: 17 July 2013 / accepted date: 26 November 2013)

The effects of Cr and Zr addition on the coarse grain surface layer in EN AW 6082 tube extrusions were
investigated. The decoration of the tube surfaces and the weld seams with coarse recrystallized grains
reflects the strain as well as the temperature gradients that predominate across the section of the tubes
during extrusion. The recrystallization resistance provided by Mn does not suffice to avoid the coarse sur-
face grains. With structural features that are almost identical to those of the base 6082 alloy, the 6082
alloy with 0.06 wt% Zr also fails to offer any improvement. The coarse grain surface layer is much thin-
ner and recrystallization is entirely avoided across the weld seams upon the addition of 0.15 wt% Cr. The
superior recrystallization resistance of the revised alloy is attributed to the increase in the population of the
Cr-rich Al(Cr,Mn,Fe)Si as well as (Al, Si)3Zr dispersoid particles. It is reasonable to conclude that the co-
addition of Zr and Cr has a favourable impact on the resistance to recrystallization of EN AW 6082 alloy.
Keywords: aluminium alloys, extrusion, recrystallization, grain growth, optical microscopy

1. INTRODUCTION eters [3]. Processing must be optimized to ensure a fibrous


structure across the section as partially recrystallized struc-
AlMgSi extrusion alloys offer a very attractive combina- tures with coarse grains, particularly at the surface, are detri-
tion of functional and mechanical properties that make them mental to strength, toughness, and formability [7-14]. A fibrous
an ideal material for a variety of light weight structural appli- grain structure improves not only strength, fatigue, and tough-
cations [1-4]. Among the several high strength alloys from ness properties [15], but also forming characteristics, surface
the ternary Al-Mg-Si system, EN AW 6082 has been receiv- quality, and corrosion resistance. Therefore, control of grain
ing a great deal of attention recently for use in automotive structure across the section is of paramount importance for
extrusions owing to its superior corrosion resistance. EN adequate performance.
AW 6082 uses an excess amount of silicon to increase the It has been reported that the addition of Zr and Sc helps to
age hardening response and manganese to control the grain retard recrystallizaton and thus to ensure fibrous grains across
structure [1]. Mn forms dispersoid particles during homoge- the section in several aluminium alloys [16-22]. While Zr
nization of the billet [3] that retard the nucleation and growth alone is not very effective, it has a very favourable impact on
of new grains during and after extrusion [5]. In contrast to the the grain structure of EN AW 6082 alloys when used together
low-strength EN AW 6060 and 6063 alloys that often exhibit with Sc [16-19]. Sc, however, is costly. It is thus of great inter-
fully recrystallized structures, extrusions produced from EN AW est to find other alloying combinations that can have a simi-
6082 alloy are frequently found to contain partially recrystal- lar impact on the recrystallization resistance. The effect of Cr
lized structures [6-8]. Coarse grains at or near the surface are and Zr addition on the grain structure of EN AW 6082 tube
common when the press exit temperature exceeds the recrys- extrusions used in suspension bushings in the automotive
tallization point of the alloy. The thickness of the peripheral industry was investigated in the present work. In particular,
coarse grain (PCG) zone may vary considerably and covers the potential of the co-addition of Zr and Cr to improve the
the entire section in the worst possible case. recrystallization resistance was explored.
Satisfying the increasing market demand for improved
performance in EN AW 6082 alloys requires precise control 2. EXPERIMENTAL PROCEDURE
of the alloy chemistry and fine tuning of the process param-
EN AW 6082 alloys were cast industrially with a state-of-
*Corresponding author: Yucel.birol@deu.edu.tr the art hot top air-slip vertical billet caster in the form of
KIM and Springer 7400 mm long, 203 mm diameter billets. The chemical com-
728 Yucel Birol

Table 1. Chemical composition of the EN AW 6082 alloys investigated in the present work
alloy Si Fe Cu Mn Mg Cr Zr Ti B
A 0.973 0.1432 0.0152 0.4004 0.560 0.0931 0.0013 0.0202 0.0013
B 1.068 0.1384 0.0107 0.4158 0.581 0.0977 0.0652 0.0238 0.0015
C 0.996 0.1139 0.0119 0.4107 0.606 0.1536 0.1357 0.0225 0.0013

positions of these billets are given in Table 1. The billets


were homogenized at 580 °C for 8 h and subsequently cooled
-1
to room temperature at a rate of 400 °Ch . The billets thus
produced were pre-heated to 500 °C. The tubes used in the
manufacture of the suspension bushings were extruded at a
-1
rate of 5.5 m.min with a welding chamber technique. The
exit temperature was fixed at 545 °C and the profiles were
rapidly cooled to room temperature. EN AW 6082 tubes thus
produced exhibit five longitudinal weld seams equally spaced
every 72 degrees and extend along the length of the tube.
Standard metallographic procedures were employed to
prepare the transverse sections of the EN AW 6082 tubes in
an attempt to identify the macro- and microstructural features.
These sections were anodised in Barker’s solution, 5 ml HBF4
(48%) in 200 ml water, and then examined with an optical
microscope under polarized light for a detailed analysis of the
grain structure across the section. Standard 3 mm TEM discs
were obtained by stamping and were subsequently ground to
a thickness of 0.12 mm. Thin foils were electrolytically pol-
ished using a Struers Tenupol 2 unit filled with a solution of
33% HNO3 in methanol at -15 °C, 14 V. A Jeol JEM 2100
LaB6 model high resolution transmission electron micro-
scope (HRTEM) operated at 200 kV and equipped with an
Oxford Instruments X-sight 6498 energy dispersive x-ray
spectroscopy (EDS) unit was employed to investigate dis-
persoid particles. An XRD analysis with CuKa radiation was
performed to identify the intermetallic phases. Very low scan-
ning rates were used to improve the counting frequency. Fig. 1. (a) Transverse section of the tube extruded from alloy A. Higher
magnification view of (b) region A and (c) region B in part (a). Arrows
3. RESULTS AND DISCUSSION indicate the weld seams.

The tube extruded from the base EN AW 6082 alloy (Alloy extrusion of hollow profiles, the material flows through the
A) exhibits a multi-layer structure across the section with portholes and is divided into several streams around the core
coarse equiaxed grains near the edges and fibrous grains in support that holds the stationary mandrel before it is welded
the interior (Figs. 1a and b). These structural features suggest together in the welding chamber [29]. The strain distribution
that the exit temperature during extrusion was just in the thus produced involves through-thickness gradients that are
neighbourhood of the recrystallization point of this alloy. cyclic around the diameter with a frequency that depends on
The coarse recrystallized grains have grown further from the die design, i.e. the number of portholes. The weld seams
both sides and cover the entire section at the weld seams are essentially mating surfaces that also experience high
(Figs. 1a and c). The weld seams appear to be more prone to strains before they are bonded in the solid-state in the welding
recrystallization than the rest of the section. chamber. The temperature at the surfaces including the weld
Large plastic strains are required to form the starting billet seams is higher than the average due to frictional heating,
into a profile in the extrusion process. Extrusion deformation which provides the highest driving force for recrystallization.
is heterogeneous and varies across the section of the profile The decoration of the tube surfaces and the weld seams
[23,24]. The shear strain increases moving away from the with recrystallized grains reflects the strain as well as the
centre of the section and peaks at the surface [25-28]. In the temperature gradients prevailing across the section of the
Effect of Cr and Zr on the Grain Structure of Extruded EN AW 6082 Alloy 729

extruded tubes (Fig. 1). Recrystallization of a volume ele-


ment occurs once it is strained to a critical level at the extru-
sion temperature. This is most likely to start at the surfaces
and the weld seams of a hollow extrusion as evidenced by
the recrystallization pattern across the section. However, the
above account only explains partially recrystallized sections
but not unusually coarse surface grains. Coarse grains in the
recrystallization regions suggest that very few of the poten-
tial nucleation sites have become potent and started to grow
once the conditions for recrystallization were attained. The
majority of sites, on the other hand, were pinned by the dis-
persoids, a characteristic feature of 6082 alloys, which inter-
acted with the progress of the recrystallization reaction [30-
33]. Sperry [34] argues that a critical stored energy condition
leading to coarse grain formation is developed if the level of
stored energy is only sufficient to enable a few potential nucle-
ation sites to become potent and to grow. A fibrous core and
peripheral coarse grains are typical in medium to high strength Fig. 2. (a) Transverse section of the tube extruded from alloy B. (b)
AlMgSi alloys, such as the 6082 alloy investigated in the Higher magnification view of the marked region in part (a). Arrows
present work, particularly when produced at a low extrusion indicate the weld seams.
ratio [35]. The transition from a fibrous to a fully recrystallized
structure is promoted by increased work of deformation, i.e.,
low billet temperatures, higher ratios, and high ram speeds [35]. Alloy B has an additional 0.06 wt% Zr and is thus expected to
The measures taken to retard recrystallization in the standard contain, in addition to Mn-bearing particles, Al3Zr disper-
EN AW 6082 alloy apparently introduce the risk of abnormal soids, because the solid solubility of Zr in aluminium is
grain growth at the same time. The Mn bearing dispersoids about 0.05 wt% at 500 °C [37]. This alloy exhibits a slightly
that are incorporated in the alloy to retard recrystallization thinner coarse grain zone at the inner and outer surfaces of
adversely affect grain features when recrystallization finally the extruded tubes. However, the coarse recrystallized grains
occurs. The preferred sites for recrystallization are shown to are still evident along the weld seams (Figs. 2a and b). It is
be the inner and outer surfaces as well as the weld seams, thus concluded that the addition of 0.06 wt% Zr offers very
which are deformed more and heated to higher temperatures limited improvement in the section grain structure. Estima-
than the rest of the section due to frictional heating. Very few tions of the area fraction of recrystallization and average
of the recrystallized nuclei can grow under these circum- grain size across and outside the weld seams provide further
stances owing to the pinning of the grain boundaries, which evidence for this modest improvement in the section features
leads to the formation of few very coarse grains. The pinning (Table 2). This is not surprising in view of the results of the
effect provided in alloy A by Mn apparently does not suffice metallographic investigations and the XRD analysis of the
to avoid recrystallization and is clearly responsible for the respective tube samples (Figs. 3, 4, and 5). The size and the
abnormally coarse surface grains. A partially recrystallized population of the particles in alloys A and B are nearly iden-
section was reported to be more detrimental to the integrity tical at overview magnifications (Fig. 3). This is confirmed
of the profile since the boundary between the fibrous and further with TEM investigations (Figs. 4a and b). The dis-
coarse grain zones is susceptible to cracking under severe persoids in alloy B were invariably found by an EDS analy-
loads [36]. On the other hand, fibrous grains would prevail if sis to be Mn-rich Al(Mn,Cr,Fe)Si particles. They were in the
all boundaries were effectively pinned. A plausible solution 100-200 nm size range with features and compositions very
then is to increase the pinning effect by increasing the amount similar to those found in alloy A (Figs. 4a and b). The intensi-
and the effectiveness of dispersoid forming elements. ties of the Bragg reflections generated by these particles are

Table 2. Area fraction and the average grain size of the recrystallized zones across and outside the weld seams
Alloy A Alloy B Alloy C
Area fraction of Across weld seam 100 100 38
recrystallization (%) Outside weld seam 45 27 13
Across weld seam 299 290 168
Average grain size (µm)
Outside weld seam 190 156 144
730 Yucel Birol

Fig. 3. Microstructural features of the tubes extruded from (a) alloy A, (b) alloy B and (c) alloy C.

Fig. 4. TEM micrographs and typical EDS analysis of dispersoid particles in tubes extruded from alloys (a) A, (b) B, and (c) C.

nearly the same in alloys A and B (Figs. 5a and b). There was fuses slowly. Furthermore, it is difficult to obtain sufficient
no evidence of Al3Zr dispersoids in alloy B. Any improve- precipitation of Al3Zr dispersoids with the desired particle
ment in its recrystallization resistance with nearly identical features [16,17,19,20,22]. Al3Zr dispersoids were reported to
microstructural features is hence highly unlikely. be absent in an Al-Mn-Zr alloy even when the microsegre-
It is fair to conclude from the foregoing that the addition of gations of Zr in an Al-Zr-Mn alloy were largely eliminated
0.06 wt% Zr is not sufficient to avoid a through thickness with a high temperature annealing treatment at 630 °C [20].
coarse grain structure across the weld seams. Control of the Zr is known to be more effective when employed with Sc
peripheral coarse grain structure in the medium to high strength owing to a uniform distribution [16,17,19,22] and to the
AlMgSi alloys with Zr addition is not an easy task. It is higher stability of Al3(ScxZr1−x) dispersoids [18]. In addition,
necessary to achieve a uniform distribution of dispersoids for the Zr concentration in the present case is lower than the Zr
Zr to be effective against recrystallization [16,17,19,20,22]. concentration that has been reported to lead to a minimum
However, it is difficult to distribute Zr homogeneously in the fraction of recrystallization in a 7XXX alloy, i.e. 0.13 wt%
cast structure because it makes a peritectic system with Al [38].
and thus segregates to the grain centres [20]. Commercial The next step was thus to increase the Zr content of the EN
homogenization cycles also fail in this respect since Zr dif- AW 6082 alloy to 0.13 wt% in order to promote the forma-
Effect of Cr and Zr on the Grain Structure of Extruded EN AW 6082 Alloy 731

Fig. 5. X-ray diffraction spectra of (a) alloy A, (b) alloy B, and (c)
alloy C.
Fig. 7. (a) TEM micrograph and (b) EDS analysis of Zr-bearing parti-
cle extruded from alloy C.

50% increase in the dispersoid population in alloy C with respect


to alloys A and B. The majority of these particles were iden-
tified by EDS analysis to be of the Al(Cr,Mn,Fe)Si variety
(Fig. 4c). They are relatively richer in Cr with respect to those
in alloy B. The diffraction lines of the ac-Al12(Cr,Mn,Fe)3Si
compound in the XRD spectrum of alloy C were much stronger
with respect to those in alloys A and B, providing further
evidence for the increase in the volume fraction of the ac-Al
(Cr,Mn,Fe)Si particles (Fig. 5c). There were also Zr-bearing
particles. These particles contained Si and were thus identi-
fied to be (Al1-xSix)3Zr (Fig. 7). (Al, Si)3Zr dispersoid particles
were found to be the most effective inhibitor of recrystalliza-
tion and decrease the rate of nucleation [21]. It is reasonable
to conclude from the foregoing that the co-addition of Zr and
Fig. 6. (a) Transverse section of the tube extruded from alloy C. (b) Cr has a favourable impact on the resistance to recrystalliza-
Higher magnification view of the marked region in part (a). Arrows tion of EN AW 6082 alloy.
indicate the weld seams.
4. CONCLUSION

tion of dispersoids (Alloy C). The Cr concentration was also The coarse recrystallized grains on the tube surfaces and
increased. The increase in the Zr and Cr concentrations pro- across the weld seams reflect the strain as well as the tempera-
duced a marked improvement in the section grain structure. ture gradients prevailing across the section of the extruded
The PCG zone is much thinner and recrystallization is largely 6082 alloy tubes. The pinning effect provided by approxi-
avoided across the weld seams in the tubes produced from mately 0.4 wt% Mn in a typical 6082 alloy apparently fails
alloy C (Fig. 6). This improvement in the recrystallization resis- to offer adequate recrystallization resistance. The improve-
tance of alloy C is evidenced also by the area fraction of ment provided with additional 0.06 wt% Zr is also very lim-
recrystallization and average grain size estimated across and ited. This is consistent with the structural features, which are
outside the weld seams (Table 2). almost identical to those of the base 6082 alloy with predom-
This improvement is attributed to a notable increase in the inantly Mn-rich cubic Al(Mn,Cr,Fe)Si particles. The coarse
population of the dispersoid particles (Figs. 3c and 4c). The grain zone is much thinner and recrystallization is largely
number densities of the dispersoid particles were estimated avoided across the weld seams when the Cr and Zr concen-
11 11 11 -2
from Fig. 3 to be 5.9.10 , 6.3.10 and 8.7.10 m for alloys trations were increased to 0.15 and 0.13 wt%, respectively,
A, B, and C, respectively. These estimations imply a nearly owing to the increase in the population of the Cr-rich
732 Yucel Birol

Al(Cr,Mn,Fe)Si as well as (Al, Si)3Zr dispersoid particles. It Aluminum Extruders Council and The Aluminum Associa-
is reasonable to conclude that the co-addition of Zr and Cr tion, Chicago, Illinois, USA (2004).
has a favourable impact on the resistance to recrystallization 15. T. Sheppard, Extrusion of Aluminium Alloys, Kluwer Aca-
of EN AW 6082 alloy. demic Publishers, USA (1999).
16. B. Forbord, H. Hallem, N. Ryum, and K. Marthinsen, Mater.
ACKNOWLEDGEMENTS Sci. Eng. A 387-389, 936 (2004).
17. J. Røyset, U. Tundal, S. R. Skjervold, G. Waterloo, C. Braathen,
It is a pleasure to thank F. Alageyik for his help in the and O. Reiso, Mater. Forum. 28, 246 (2004).
metallographic analysis of samples and Dr. O. Duygulu for 18. B. Forbord, L Auran, W. Lefebvre, H. Hallem, and K. Marthin-
the TEM investigations. sen, Mater. Sci. Eng. 424, 174 (2006).
19. Y. W. Riddle, H. Hallem, and N. Ryum, Mater. Sci. Forum
396-402, 563 (2002).
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