Journal of Alloys and Compounds 354 (2003) 216–220 L

www.elsevier.com / locate / jallcom

Effect of ECAP on microstructure and mechanical properties of a

commercial 6061 Al alloy produced by powder metallurgy
a, b c b
Si-Young Chang *, Ki-Seung Lee , Seung-Hoe Choi , Dong Hyuk Shin
a
Department of Materials Engineering, Hankuk Aviation University, 200 -1 Hwajon-dong, Koyang-shi, Kyunggi-do 412 -791, South Korea
b
Department of Metallurgy and Materials Science, Hanyang University, Ansan, Kyunggi-do 425 -791, South Korea
c
Department of General Studies, Hankuk Aviation University, Koyang-shi, Kyunggi-do 412 -791, South Korea
Received 15 January 2002; received in revised form 7 May 2002; accepted 29 October 2002

Abstract

The 6061 (Al–1.01 wt% Mg–1.07 wt% Si) Al alloy was fabricated by powder metallurgy, and then subjected to equal channel angular
pressing. The microstructure and mechanical properties such as microhardness and tensile properties of the equal channel angular pressed
P/ M 6061 Al alloy were investigated. The P/ M 6061 Al alloy had an initial grain size of approximately 20 mm. After two pressings at
373 K using route A, the sample revealed microstructure of subgrain bands with a length of |0.8 mm and a width of |0.3 mm. The
subgrain bands became larger above 1 mm in length and width after two pressings at 573 K. An equiaxed ultra-fine grained structure with
the mean grain size of |0.5 mm was obtained after four repetitive equal channel angular pressings at 473 K using route A and C. The
microhardness of P/ M 6061 Al alloys was drastically increased from about 40 to 80 Hv by two repetitive pressings at 373 K. However,
the microhardness decreased with increasing the pressing temperature. The tensile strength of 6061Al alloy before the equal channel
angular pressing was 95 MPa, whereas it increased to both 248 MPa after two pressings at 373 K and 130 MPa after four pressings at 473
K, which was superior to that of a commercial 6061-O Al alloy.
 2003 Elsevier Science B.V. All rights reserved.

Keywords: Ultra-fine grained Al–Mg–Si alloy; Powder metallurgy; Equal channel angular pressing; Mechanical properties

1. Introduction and excellent corrosion resistance, weldability, and fatigue

According to a number of recent research studies, the
equal channel angular pressing (ECAP) [1–5] has received
much attention as an attractive method to obtain a sub-
micrometer ultra-fine grained (UFG) structure in a variety
of bulk metallic materials without residual porosity: for
example, Armco iron [6,7], Al alloys and their composites
[8–12], Cu [13–16], Mg alloys [8], pure Ni [6], low
carbon steel [4,5,17–20], Ti alloys [21–23], and Zn–22%
Al [24].
Among Al alloys, a commercial 6061 Al alloy which is
one of Al–Mg–Si system alloys, has been widely used as
structural material for construction and transportation such
as vessels and automobile, because it has medial strength
*Corresponding author. Tel.: 182-2-300-0168; fax: 182-2-3158-3770.
E-mail address: sychang@mail.hau.ac.kr (S.-Y. Chang).
strength [25]. However, this alloy is basically used in the
type of as-cast, except only a portion used as wrought
material due to its poor workability. In order to improve
the poor workability, the powder metallurgy can be
adopted in the step of processing because of its several
merits that are possible to reduce the compounds occurring
during solidification and to obtain the fine grained structure
compared with as cast materials [26]. In addition, follow-
ing the powder metallurgy, the subsequent processes such
as rolling, extrusion and forging are generally conducted to
improve the mechanical properties. Accordingly, it is very
much of interest to apply the ECAP as the subsequent
process of a commercial 6061 Al alloy produced by
powder metallurgy.
In this study, therefore, a commercial 6061 Al alloy was
prepared by the powder metallurgy and then the micro-
structure and mechanical properties at room temperature
after obtaining the UFG structure of P/ M 6061 Al alloy by
ECAP was evaluated.

0925-8388 / 03 / $ – see front matter  2003 Elsevier Science B.V. All rights reserved.
doi:10.1016 / S0925-8388(03)00008-2
 S.-Y. Chang et al. / Journal of Alloys and Compounds 354 (2003) 216–220
2. Experimental procedure
Air atomized 6061 Al alloy (Al–1.01% Mg–1.07%
Si–0.35% Cu–0.25% Fe–0.05% Mn–0.12% Cr (in wt%))
powders with a size below 30 mm were prepared. The
powders were hot-pressed at 773 K with a pressure of 100
MPa under a vacuum atmosphere of approximately 1 Pa.
The hot-pressed samples with a dimension of [32380
mm were machined to cylindrical samples of [10380 mm
as pre-materials for ECAP. The ECAP was carried out at
373–573 K. The present ECAP die was designed to yield
an effective strain of |1 by a single pass: the inner angle
and the arc of curvature at the outer point of contact
between channels of the die were 90 and 208, respectively
[27,28]. During the ECAP, the samples were pressed
repetitively using two processing routes: route A in which
the sample is repetitively pressed without any rotation and
route C in which the sample is rotated 1808 around its
longitudinal axis between individual pressings [11].
Tensile tests were performed using an Instron machine
on the tensile specimens with 10 mm in gauge length at the
initial strain rate of 1.00310 23 s 21 and at room tempera-
ture. Microhardness was measured using a Vickers mi-
crohardness tester at a load of 0.05 kg for 15 s. Micro-
structure examination of samples before / after ECAP was
carried out using a field emission scanning electron
microscope (FE-SEM, JSM6330F, Jeol, Japan) and a
transmission electron microscope (TEM, Jeol 2010, Japan)
operated at 200 keV. The microstructure of x-plane and
y-plane in samples before / after ECAP was observed;
where the x-plane is the plane perpendicular to the
longitudinal axis of the sample and the y-plane denotes the
side-viewed plane parallel to the longitudinal axis of the
sample.
Fig. 1. (a) Microstructure of as hot-pressed 6061 Al alloy before ECAP and (b) EDS analysis of a particle at a grain boundary.
217
3. Results
3.1. Microstructural characteristics
Fig. 1 shows microstructure and EDS analysis of P/ M
6061 Al alloys before ECAP. The grains have a size of
approximately 20 mm. The particles which existed in the
grain boundary were identified as Si by EDS analysis. In
this study, however, the compounds such as Mg 2 Si and
AlFeSi that are generally included in cast 6061 Al alloy
[29] were not detected.
The microstructure of the ECA pressed P/ M 6061 Al
alloy are shown in Fig. 2. After ECAP, the initial grain
boundaries were hardly identified, and the Si particles were
uniformly distributed. The sample pressed at relatively low
temperature of 373 K showed that the Si particles were
slightly aligned to flow direction. However, the phenom-
enon disappeared with increasing pressing temperature.
This is because the magnitude of shear deformation in
metallic materials during ECAP is closely related to the
pressing temperature [30,31]. In addition, it is apparent
that the particles are well-distributed with increasing
pressing temperature. On the other hand, there is no
microstructural difference in the samples pressed using
route A and route C (Fig. 2c and d).
Fig. 3 represents TEM micrographs of ECA pressed
P/ M 6061 Al alloy. After two pressings at 373 K using
route A, the elongated grains with a length of |0.8 mm and
a width of |0.3 mm were observed. The SAED pattern
showed the appearance of the diffused spots and the extra
spots, indicating the formation of a high angle boundary.
In contrast, the grains after two pressings at relatively high
temperature of 573 K became larger above 1 mm in length
and width. The corresponding SAED pattern was char-
218 S.-Y. Chang et al. / Journal of Alloys and Compounds 354 (2003) 216–220
Fig. 2. Microstructure of 6061 Al alloys after ECAP: (a) and (b) two pressings at 373 and 573 K, respectively, using route A; (c) and (d): four pressings at
473 K using route A and C, respectively.
acterized by relatively clear spots. This implies that most
of the boundaries in the grains formed by two pressings
would be low-angled. Near equiaxed ultra-fine grains
approximately 0.5 mm in grain size were obtained by four
repetitive ECAPs. However, no difference in microstruc-
ture according to the route was observed. In addition, the
number of rings in the SAED pattern increased and the
spots became more diffused compared with samples after
two ECAPs at 373 and 573 K.
3.2. Mechanical properties
The microhardness of ECA pressed P/ M 6061 Al alloy
is shown in Table 1. The microhardness revealed a
substantial increase after the ECAP. In particular, there was
a significant change in the microhardness after the pressing
at 373 K. The increase of the pressing temperature resulted
in the small increase of microhardness. However, there
was no change according to the difference of route. In
addition, the microhardness between the x-plane and the
y-plane had same tendency to increase after the pressing.
The drastic increase of microhardness after the pressing is
because of the work hardening that is caused by the
formation of sub-micrometer ordered grains and the den-
sity increase of dislocation occurring with the shear
deformation in the initial grain interior. Additionally, the
reason why the microhardness decreases with increasing
the pressing temperature is deduced to be due to the
dynamic recovery occurring during the pressing [28] at
higher temperatures.
Table 2 shows the variation of the tensile strength and
elongation of P/ M 6061 Al alloy after the ECAP, together
with the commercial 6061 Al alloys. The tensile strength
of hot-pressed 6061 Al alloy drastically increased from 95
to 248 MPa after two pressings at 373 K. In contrast, after
four repetitive ECAPs at 473 K, the tensile strength
increases to 130 MPa and the elongation is 25%. Addition-
ally, the P/ M 6061 Al alloy pressed repetitively at 573 K
revealed low tensile strength and elongation. These results
are well compatible with both the microstructural charac-
teristics shown in Fig. 3 and the recent report [30,31].
From the above results, it is apparent that the improvement
of tensile strength is attributable to the grain refining by
the ECAP process. On the other hand, there was no
difference in tensile properties with the route.
Additionally, Table 2 compares the tensile strength and
elongation of the ECA pressed P/ M 6061 Al alloy to the
same values for both the commercial fully-annealed 6061-
O and T4 treated 6061 available [32]. The tensile strength
of two repetitively ECA pressed P/ M 6061 Al alloy at 373
 S.-Y. Chang et al. / Journal of Alloys and Compounds 354 (2003) 216–220 219

Fig. 3. TEM micrographs of the ECA pressed P/ M 6061 Al alloys: (a) and (b) two pressings at 373 and 573 K, respectively, using route A; (c) and (d) four
pressings at 473 K using route A and C, respectively.

Table 1 over the fully annealed 6061-O alloy without decrease in

Microhardness (Hv) of the ECA pressed P/ M 6061 Al alloys (Hv)
elongation. According to recent reports, it has a close
x-plane y-plane relation to the annihilation kinetics of extrinsic grain
As-received 39 46 boundary dislocation introduced by severe plastic deforma-
Two pressings at 373 K (route A) 82 79 tion and the number of dislocations necessary to deform
Two pressings at 573 K (route A) 54 55 the ultra-fine grain [13,33,34].
Four pressings at 473 K (route A) 65 65
Four pressings at 473 K (route C) 67 65

4. Summary
K is nearly two times higher than that of the fully annealed
6061-O alloy and was comparable to that of the T4 treated
1. The ECAP was successfully conducted at various
6061 T4 alloy, whereas the elongation decreases. In
temperatures and two different routes on the same
contrast, there was a slight increase in tensile strength of
sample up to a total of four pressings through the die
P/ M 6061 Al alloy after four repetitive pressings at 473 K
such that the sample was not rotated (route A) and
Table 2
Tensile properties of the ECA pressed P/ M 6061 Al alloys and the commercial 6061 Al alloys
Tensile strength Elongation
(MPa) (%)
As-received P/ M 6061 95 8
Two ECA pressed P/ M 6061 (373 K, route A) 248 10
Two ECA pressed P/ M 6061 (573 K, route A) 90 18
Four ECA pressed P/ M 6061 (473 K, route A) 130 25
Four ECA pressed P/ M 6061 (473 K, route C) 130 25
6061-O 123 25
6061-T4 235 22
220 S.-Y. Chang et al. / Journal of Alloys and Compounds 354 (2003) 216–220
rotated 1808 (route C) around its longitudinal axis
between pressings.
2. After two ECAPs at 373 K using route A, the sample
revealed microstructure of subgrain bands with a length
of |0.8 mm and a width of |0.3 mm. The subgrain
bands became larger above 1 mm in length and width
after two ECAPs at 573 K. An equiaxed ultra-fine
grained (UFG) structure with the mean grain sizes of
|0.5 mm was obtained after four repetitive ECAPs
using route A and C.
3. The microhardness and tensile strength increased with
decreasing the pressing temperature. The microhardness
of sample after four repetitive ECAPs at 473 K was
approximately 20 Hv higher in microhardness than that
of as-received one. The tensile strength of P/ M 6061 Al
alloy increased from 95 MPa to 248 MPa after two
ECAPs at 373 K and 130 MPa after four pressings at
473 K, which was superior to that of a fully annealed
6061-O Al alloy.
4. The ECAP technique can be effectively applied as the
subsequent process of a commercial 6061 Al alloy
produced by powder metallurgy. In particular, many
repetitive pressings at low temperatures (,1 / 2 T m ) are
sufficient to give the ultrafine grained (UFG) structure
resulting in the highly increased microhardness and
tensile strength.
Acknowledgements
This work was supported by the ‘National Research
Laboratory Program’ of Korea Ministry of Science and
Technology.
References
[1] R.Z. Valiev, R.K. Islamgaliev, I.V. Alexandrov, Prog. Mater. Sci. 45
(2000) 103.
[2] D.H. Shin, Y.S. Kim, E.J. Lavernia, Acta Mater. 49 (2001) 1.
[3] D.H. Shin, I.Y. Kim, J. Kim, K.T. Park, Acta Mater. 49 (2001) 1285.
[4] D.H. Shin, B.C. Kim, K.T. Park, W.Y. Choo, Acta Mater. 48 (2000)
3245.
[5] D.H. Shin, B.C. Kim, Y.S. Kim, K.T. Park, Acta Mater. 48 (2000)
2247.
[6] V.M. Segal, Mater. Sci. Eng. A 197 (1995) 157.
[7] R.Z. Valiev, Yu.V. Ivanisenko, E.F. Rauch, B. Baudelet, Acta Mater.
44 (1996) 4705.
[8] M.V. Markshev, C.C. Bampton, M.Yu. Murashkin, D.A. Hardwick,
Mater. Sci. Eng. A 234–236 (1997) 927.
[9] R.Z. Valiev, A.V. Korznikov, R.R. Mulyukov, Mater. Sci. Eng. A 168
(1993) 141.
[10] P.B. Berbon, N.K. Tsenev, R.Z. Valiev, M. Furukawa, Z. Horita, M.
Nemoto, T.G. Landon, Metall. Mater. Trans. A 29 (1998) 2237.
[11] Y. Iwahashi, M. Furukawa, Z. Horita, M. Nemoto, T.G. Langdon,
Metall. Mater. Trans. A 29 (1998) 2245.
[12] R.Z. Valiev, R.K. Islamgaliev, N.F. Kuzmina, Y. Li, T.G. Langdon,
Scripta Mater. 40 (1999) 117.
[13] R.Z. Valiev, E.V. Kozlov, Yu.F. Ivanov, J. Lian, A.A. Nazarov, B.
Baudelet, Acta Metall. Mater. 42 (1994) 2467.
[14] S. Ferrasse, V.M. Segal, K.T. Hartwig, R.E. Goforth, Metall. Mater.
Trans. A 28 (1997) 1047.
[15] R.Z. Valiev, I.V. Alexander, Nanostruct. Mater. 12 (1999) 35.
[16] I.V. Alexander, R.Z. Valiev, Nanostruct. Mater. 12 (1999) 709.
[17] D.H. Shin, K.H. Oh, W.J. Kim, S.W. Lee, W.Y. Choo, J. Korean Inst.
Metall. Mater. 37 (1999) 1048.
[18] D.H. Shin, W.J. Kim, W.Y. Choo, Scripta Mater. 41 (1999) 259.
[19] D.H. Shin, C.W. Seo, J.R. Kim, K.T. Park, W.Y. Choo, Scripta Mater.
42 (2000) 695.
[20] K.T. Park, Y.S. Kim, J.K. Lee, D.H. Shin, Mater. Sci. Eng. A 293
(2000) 165.
[21] S.L. Semitan, V.M. Segal, R.E. Goforth, N.D. Frey, D.P. DeLo,
Metall. Mater. Trans. A 30 (1999) 1425.
[22] D.P. DeLo, S.L. Semitan, Metall. Mater. Trans. A 30 (1999) 2473.
[23] S.L. Semitan, D.P. DeLo, Mater. Design 21 (2000) 311.
[24] M. Furukawa, Y. Ma, Z. Horita, M. Nemoto, R.Z. Valiev, T.G.
Langdon, Mater. Sci. Eng. A 241 (1998) 122.
[25] Japan Institute of Light Metals, Microstructure and Properties of
Aluminum Alloys, 1991, pp. 290–291.
[26] R.M. German, Powder Metallurgy of Iron and Steel, Wiley, New
York, 1998, pp. 380–385.
[27] K. Nakashima, Z. Horita, M. Nemoto, T.G. Langdon, Acta Mater.
46 (1998) 1589.
[28] Y. Iwahashi, J. Wang, Z. Horita, M. Nemoto, T.G. Langdon, Scripta
Mater. 35 (1996) 143.
[29] Japan Institute of Light Metals, Microstructure and Properties of
Aluminum Alloys, 1991, pp. 279.
[30] D.H. Shin, Y.K. Kim, K.T. Park, Y.S. Kim, Mater. Sci. Eng. (2001)
in press.
[31] A. Yamashita, D. Yamaguchi, Z. Horita, T.G. Langdon, Mater. Sci.
Eng. A 287 (2000) 100.
[32] Japan Institute of Light Metals, Microstructure and Properties of
Aluminum Alloys, 1991, p. 478.
[33] J. Lian, B. Baudelet, A.A. Nazarov, Mater. Sci. Eng. A 172 (1993)
23.
[34] W. Lojkowski, Acta Metall. Mater. 39 (1991) 1891.