JMPT

You might also like

Download as pdf or txt
Download as pdf or txt
You are on page 1of 6

Journal of Materials Processing Technology 182 (2007) 363368

Influence of cold extrusion on the microstructure and mechanical


properties of an aluminium alloy previously subjected to
equal channel angular pressing
D. Nagarajan, Uday Chakkingal , P. Venugopal
Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036, India
Received 13 June 2006; received in revised form 4 August 2006; accepted 21 August 2006

Abstract
Severe plastic deformation processes like the equal channel angular pressing (ECAP) process are currently the subject of extensive investigation
and it has been established that ECAP is capable of producing ultrafine grained microstructures in Al alloys. However, practical applications of
ECAP process will depend upon the advantages obtained when this process is combined with conventional forming techniques. In the current study,
the advantages of the equal channel angular pressing (ECAP) process, when used as an intermediate processing step prior to conventional forming
by cold extrusion, have been investigated. ECAP of Al alloy AA 6101 was carried out using a die with 105 die angle for three passes through
two different processing routes and these specimens were subsequently processed through conventional cold extrusion. Mechanical property and
microstructure data show that improved properties after cold extrusion are heavily dependent upon prior ECAP processing routes. Implications of
the results for the processing of ultrafine grained materials are discussed.
2006 Elsevier B.V. All rights reserved.
Keywords: Severe plastic deformation; Equal channel angular pressing; Ultrafine grained microstructure; Aluminium alloys

1. Introduction
There has been increasing interest in bulk ultrafine grained
materials as they exhibit superior mechanical properties such
as high strength with enhanced ductility, high yield stress and
improved toughness [1,2]. An important technique for producing ultrafine grained materials in bulk form is the equal channel
angular pressing (ECAP) [3,4]. In principle, the ECAP die consists of two intersecting channels of equal cross section that
meet at a predetermined angle 2 (which is usually between 90
and 135 ). The work piece is inserted into the top channel and
extruded through the bottom channel with the help of a punch.
The process can be repeated a number of times using the same
die, because the cross sectional dimensions of the workpiece
do not change before and after processing. By changing the
orientation of the billet between consecutive passes and thereby
changing the strain path of the deformation, different microstructures and mechanical properties can be produced [57]. Fig. 1
shows a schematic diagram of an ECAP die.

Corresponding author. Tel.: +91 44 2257 4775; fax: +91 44 2257 4752.
E-mail address: udaychak@iitm.ac.in (U. Chakkingal).

0924-0136/$ see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2006.08.016

This process has been applied to a wide variety of commercially used materials such as aluminium, copper, steel, nickel,
composites, intermetallics and powder samples [5,810]. Extensive research has been carried out on the microstructure development and mechanical property evolution during the ECAP
process. It is well known that ECAP of aluminium alloys leads
to ultrafine grained structures with improved mechanical properties. However the effects of ECAP on properties and microstructure after subsequent processing by conventional forming operations have not been widely investigated. This aspect is important because commercial applications of the ECAP process will
depend heavily on the advantages obtained when it is used as an
intermediate forming operation to produce feedstock for subsequent forming by conventional techniques.
The aim of the present work is to study the applicability of
using ECAP as an intermediate processing step before specimens are processed further through conventional cold extrusion.
In effect, the ECAP process was used to produce an ultrafine
grained specimen, which was then subjected to conventional
cold extrusion. Previously, improvements in mechanical properties in a cold extruded AA6101 alloy following ECAP using
a 120 die have been reported [11]. In the current study, the
influence of cold extrusion following ECAP of AA 6101 using

364

D. Nagarajan et al. / Journal of Materials Processing Technology 182 (2007) 363368


Table 1
Maximum pressing pressures recorded for different processing routes of ECAP
and ECAP followed by conventional extrusion

Fig. 1. Schematic diagram illustrating the ECAP process.

a 105

die on mechanical properties has been investigated. This


is because a 105 die gives more intense strain per pass as
compared to a 120 angle die (0.88 as opposed to 0.67). The
mechanical properties and microstructure resulting from different processing routes were determined. Comparisons were
made between properties resulting from specimens directly subjected to conventional cold extrusion and specimens subjected to
cold extrusion after various ECAP passes. Implications of these
results on using ECAP as an intermediate processing step prior
to conventional forming are discussed.

2. Experimental procedure
Aluminium alloy AA 6101 (composition of 0.39% Si, 0.44% Mg, 0.49% Fe,
0.002% Cu, 0.004% Mn, 0.007% Zn, balance Al) was used in this investigation.
The alloy was solution annealed at 510 C for 1 h and immediately quenched
in water. Specimens of 19.8 mm diameter and 105 mm height with a taper of
45 at one end (to facilitate easy start of ECAP) were prepared. A 105 channel
angle die (2 = 105 ), which imparts 0.88 equivalent plastic strain per pass to
the sample, was used for ECAP. The die had a sharp corner, i.e., a corner angle
of 0 . The equivalent plastic strain per pass is given by Segal et al. [3] as
2
= cot
3
where is the equivalent plastic strain imparted per pass. 2 is the channel angle
(angle between the two intersecting channels.
Pressing was carried out for three passes using two different processing
routes: route A (no rotation of the sample between consecutive passes) and route
C (180 rotation of the sample about its longitudinal axis between consecutive
passes) with molybdenum disulphide as the lubricant. The extrusion was carried
out with an average strain rate of 0.4 s1 . Specimens have been designated as 2A,
etc. where 2 represents the total number of extrusion passes and A represents the
processing route. Conventional cold extrusion was carried out on solutionized,
pass 1, 2A and 2C ECAP subjected samples. A conventional extrusion die that
imparts a strain of 0.78 was selected, which is almost equivalent to the strain
imparted by the ECAP die in a single pass. Conventional extrusion was carried
out at an average strain rate of 0.02 s1 . During extrusion, the force-stroke data
was recorded using a data acquisition system.
Tensile specimens with a gauge section of 4 mm in diameter and 20 mm
in length were made as per ASTM E-8M standards from solutionized, ECAP
processed, and conventionally extruded samples. Ultimate tensile strength and
% elongation to failure were measured. Vickers hardness measurements were
made in both perpendicular and parallel direction to extrusion using a load of
2 kg and reported as mean of ten readings. Transmission electron microscopy
was used to examine the microstructure. Specimens for TEM investigations were
prepared by twin jet electro polishing using a solution of 20% perchloric acid
+80% methanol at a temperature of 40 C. Grain sizes were measured using
the linear intercept method.

Processing route

Maximum pressing pressure (MPa)

Pass 1
Pass 2A
Pass 2C
Pass 3A
Pass 3C
CE of solutionized sample
Pass 1 ECAP + CE
Pass 2A ECAP + CE
Pass 2C ECAP + CE

320
350
344
381
420
235
287
423
420

3. Results and discussion


3.1. Pressing pressures
An initial peak pressure was observed during the ECAP of this
alloy for all processing routes except for pass 1 ECAP, where the
extrusion pressure increased continuously with stroke. Table 1
summarizes the maximum pressing pressures for different processing routes of ECAP and conventional extrusion.
It can be observed that the ECA pressing pressure increased
from one pass to another for both the processing routes. Pressure
required depends not only on the imposed strain, strain rate, and
temperature of the process, but also on the orientation of micro
shear bands and slip systems with respect to the macroscopic
shear planes. Pressing pressure required for route C of ECAP
is higher than route A, which may be due to the changes in
strain path that increase the interaction between dislocations on
intersecting slip planes. This increase in pressure is similar to
the increase in maximum load reported by Horita et al. [12]
during ECAP of Al alloys 1100 and 3004 for both routes. Higher
pressures were required for the conventional extrusion of pass
2A and 2C ECAP subjected specimens.
3.2. Hardness
Table 2 summarizes the hardness values with total strain
imparted to the sample for various processing routes of ECAP
and conventional cold extrusion. In the solutionized condition,
the alloy had a hardness of 44 HV2. ECAP through route A
Table 2
Vickers hardness values with total strain () imparted to the sample for various
processing routes of ECAP and conventional cold extrusion
Processing route

ECAP
Route A
Route C
Conventional extrusion (CE)
of solutionized sample
Pass 1 ECAP + CE
Pass 2 route A ECAP + CE
Pass 2 route C ECAP + CE

Vickers hardness number


= 0.88

= 1.76

= 2.64

84
84

86
100

95
104

93
96
93
98

D. Nagarajan et al. / Journal of Materials Processing Technology 182 (2007) 363368

365

Table 3
Values of ultimate tensile strength and elongation to failure with total strain for various processing schedules of ECAP and conventional cold extrusion
Processing route

ECAP
Route A
Route C
Conventional extrusion (CE)
of solutionized sample
Pass 1 ECAP + CE
Pass 2 route A ECAP + CE
Pass 2 route C ECAP + CE

= 0.88

= 1.76

= 2.64

UTS (MPa)

% Elongation to failure

UTS (MPa)

% Elongation to failure

UTS (MPa)

% Elongation to failure

256
256

17
17

307
329

15
16

284
297

14
14

270

19
345

16
335
334

14
14

resulted in hardness of 84, 86 and 95 HV2, respectively, after


passes 1, 2 and 3. On the other hand, on pressing through route C,
the hardness increased substantially to 100 HV2 after 2nd pass
of route C and 104 HV2 after the third pass. This is because the
rotation of the specimen by 180 between consecutive passes
increases the dislocation interactions on intersecting slip planes
[11].
Hardness value of 93 was observed after conventional cold
extrusion of solutionized specimens. Conventional cold extrusion carried out on passes 1 and 2A ECAP subjected specimens
resulted in slight increase in the hardness. Hardness remained
nearly the same after conventional extrusion of pass 2C ECAP
subjected specimens.
3.3. Tensile strength and elongation at fracture
Table 3 summarizes the values of ultimate tensile strength
and % elongation to failure with total strain for various pro-

cessing schedules of ECAP and conventional cold extrusion.


Ultimate tensile strength and % elongation to failure of the initial solutionized material were 99 MPa and 28%, respectively.
When this solutionized material was subjected to ECAP, UTS
increased remarkably up to two passes for both the processing
routes; 99 MPa to 307 MPa for route A and 99329 MPa for
route C. The % elongation to failure decreased from 28 to 15%
for route A and 16% for route C. Strength decreased after the
third pass for both the processing routes A (307 MPa after second
pass to 284 MPa after third pass) and C (329 MPa after second
pass to 297 MPa after third pass) of ECAP. This is due to the
disruption and dissolution of the original dislocation cell structure, which leads to a reduction in work hardening [13]. This
results in the decrease in the volume fraction of cell structures
and dislocation density, which cause an increase in the mean free
path of dislocations. This trend is in line with previous results
obtained during ECAP with a 120 die [11]. This is also supported by TEM micrographs shown in Fig. 2(a)(f). Fig. 2(c)

Fig. 2. TEM micrographs of specimens processed through various processing schedules of ECAP: (a) solutionized; (b) pass 1; (c) pass 2, route A; (d) pass 2, route
C; (e) pass 3, route A; (f) pass 3, route C.

366

D. Nagarajan et al. / Journal of Materials Processing Technology 182 (2007) 363368

(microstructure after pass 2 route A) and Fig. 2(d) (microstructure after pass 2 route C) show a clear dislocation cell structure
which was reinforced during the new deformation mode. However, Fig. 2(e) (microstructure after pass 3 route A) and Fig. 2(f)
(microstructure after pass 3 route C) show a partially dissoluted
dislocation cell structure with an apparent lower dislocation density. The % elongation to failure decreased from 16% to 14%
after 3rd pass for both the processing routes.
Processing by route C gave higher mechanical properties as
compared to processing by route A. This is in contrast to most
of the previous work in which processing by route A resulted in
higher strengths [5,12,14]. However, it should be noted that all
these previous investigations used a die angle, 2 = 90 . Such
an angle leads to reversal of shear during successive passes by
route C along the macroscopic plane of shear. This leads to dislocation annihilation and somewhat lower strengths after route
C processing compared to processing by route A. However, the
current study was carried out using a die angle of 105 . Therefore, strain reversal during successive passes by route C does not
occur. On the other hand, the macroscopic shear planes intersect
each other at a finite angle for a 105 die. Therefore for die angles
greater than 90 , route C processing can lead to higher strengths.
The shearing characteristics and the macroscopic shear planes
involved during ECAP and their variation with processing routes
have been investigated by Furukawa et al. [15] and Valiev et al.

[16]. Because there is a change in strain path, there may be an


initial shortage of mobile dislocations in newly activated slip
systems and this can result in an increase in strength [17]. This
is also supported by the fact that extrusion pressures for processing by route C are consistently higher than that for route
A.
Conventional extrusion carried out on solutionized specimens
resulted in UTS of 270 MPa and % elongation to failure of 19%.
Conventional cold extrusion of passes 1, 2A and 2C ECAP processed specimens showed increase in strength compared to prior
ECAP deformed condition, due to the continuous reinforcement
of dislocation cell structure that was created in the previous
deformation step. At an identical level of strain, the % elongation to failure is the same for materials processed through ECAP
and ECAP followed by conventional extrusion. This implies that
the processing route does not have a significant influence on
the % elongation to failure of the material. Highest strength of
345 MPa was obtained for specimens subjected to pass 1 ECAP
followed by conventional cold extrusion.
3.4. Microstructural characteristics
Fig. 2 shows the TEM micrographs of the ECAP subjected samples processed through various routes. The grain size
of the initial solutionized material was approximately 15 m.

Fig. 3. TEM micrographs obtained after conventional extrusion of: (a) solutionized; (b) pass 1 ECAP; (c) pass 2A ECAP; (d) pass 2C ECAP specimens.

D. Nagarajan et al. / Journal of Materials Processing Technology 182 (2007) 363368

After first pass, the grain size was reduced to 0.58 m and
it consisted mainly of parallel bands of elongated subgrains
(Fig. 2(b)). After second pass, the grain sizes were approximately 0.5 m for both processing routes (Fig. 2(c) and (d),
respectively). After third pass, the grain sizes were about the
same (Fig. 2(e) and (f), respectively), but dissoluted dislocation cell structure with lower dislocation density was observed.
This is also reflected in mechanical properties in the form of a
decrease in tensile strength from second to third pass for both
the processing routes. Relative misorientations between adjacent
grains/subgrains were not measured in this study.
Conventional extrusion carried out on solutionized samples
showed an average grain size of 0.59 m. There was no further
grain refinement observed during cold extrusion of passes 1, 2A
and 2C ECAP processed specimens. Though aluminium and its
alloys undergo grain refinement initially with increasing deformation, these values normally stabilize in the submicron range
with further deformation not leading to grain refinement. Typical microstructures after ECAP followed by cold extrusion are
shown in Fig. 3.
3.5. ECAP as a deformation step prior to conventional cold
extrusionenhancement in mechanical properties
When ECAP is used an intermediate processing step to produce specimens for subsequent cold extrusion, it is observed
from Table 3 that increases in mechanical properties are obtained
with only a slight decrease in % elongation at failure. Conventional cold extrusion of a solutionized specimen resulted in an
UTS of 270 MPa, hardness of 93 HV2 and elongation at fracture of 19%. However after cold extrusion using a specimen that
had been subjected to one pass of ECAP, the strength increased
to 345 MPa, hardness increased to 96 HV2 while elongation at
fracture decreased only slightly to 16%. The fine grains resulting
from ECAP helped to maintain a good ductility even after significant straining from cold extrusion. This implies that ECAP
can be used as a prior deformation step to conventional extrusion
for property enhancement in the cold extruded AA6101 alloy.
However what is significant is that subjecting the specimens initially to two passes of ECAP prior to cold extrusion
did not result in further improvements in mechanical properties of the cold extruded specimen. On the contrary, as shown
in Table 3, processing through two passes by ECAP followed
by cold extrusion resulted in lower mechanical properties of the
extruded product (lower UTS of 335 MPa and lower % elongation of 14% at failure) compared to specimens subjected to
only one pass of ECAP prior to cold extrusion. This implies that
additional plastic deformation by ECAP to produce a stronger
material has not resulted in any benefit as far as the cold extruded
product mechanical properties are concerned. This is obviously
because, with further strain and depending on the strain path,
some amount of strain softening can occur.
In a previous study, when ECAP was carried using a die angle
of 120 , improved cold extruded properties were obtained for
specimens subjected to larger number of ECAP passes [11]. This
is because the choice of the ECAP die angle determines the strain
imparted to the specimen per pass. From previous studies, it is

367

well known that imparting higher strain per pass (through use
of die angles closer to 90 ) is more conducive to the production
of an ultrafine grained microstructure with a large proportion of
high angle grain boundaries [16,18]. In addition, the choice of
die angle also determines the strain path and the extent of strain
reversal between successive passes for the various processing
routes. It can be expected that different results may be obtained
if ECAP is carried out using a 90 die before cold extrusion.
This has certain implications with regard to commercialization of ECAP. If ECAP is used as an intermediate processing
step to produce feedstock material which is to be later processed by conventional forming techniques like forging, extrusion, drawing, etc., high levels of severe plastic deformation
(SPD) strains may not always translate into a product with optimum mechanical properties. Levels of optimum SPD strain to
be imparted to the feedstock may have to be decided based on
the ECAP die angle used and the subsequent processing route to
be employed. The SPD microstructure obtained by ECAP can
therefore be regarded as inherently unstable and susceptible to
flow softening depending on strain paths encountered in further
processing.
4. Conclusions
Intermediate processing by ECAP to one pass followed by
conventional extrusion leads to enhanced mechanical properties
in the extruded specimens with only a small reduction in ductility. Conventional cold extrusion after ECAP did not result in
further grain refinement. ECAP can effectively be used as an
intermediate processing step prior to conventional cold extrusion for property enhancement in the cold extruded Al alloy
AA6101. Additional plastic deformation through two passes to
produce a stronger material did not result in any benefit as far as
the cold extruded product mechanical properties are concerned.
High levels of SPD strain imparted to the specimen or feedstock
may not always yield optimum mechanical properties after subsequent forming operations. Therefore optimum levels of SPD
strain may have to be decided based on the ECAP die angle used
and subsequent forming techniques to be employed.
Acknowledgements
This work was carried out as part of a research project sponsored by Department of Science and Technology, Government
of India and this assistance is gratefully acknowledged.
References
[1] R.Z. Valiev, Y.D. Vishnyakov, R.R. Mulyukov, G.S. Fainshtein, On the
decrease of Curie temperature in submicron-grained nickel, Phys. Status
Solidi A: Appl. Res. 117 (1990) 549553.
[2] R.Z. Valiev, A.V. Korznikov, R.R. Mulyukov, Structure and properties of
ultrafine grained materials produced by severe plastic deformation, Mater.
Sci. Eng. A 168 (1993) 141148.
[3] V.M. Segal, V.I. Reznikov, A.E. Drobyshevskiy, V.I. Kopylov, Plastic working of metals by simple shear, Russ. Metall. 1 (1981) 99105.
[4] R.Z. Valiev, R.K. Islamgaliev, I.V. Alexandrov, Bulk nanostructured materials from severe plastic deformation, Prog. Mater. Sci. 45 (2000) 103189.

368

D. Nagarajan et al. / Journal of Materials Processing Technology 182 (2007) 363368

[5] S. Ferrasse, V.M. Segal, K.T. Hartwig, R.E. Goforth, Microstructure and
properties of copper and aluminum alloy 3003 heavily worked by equal
channel angular extrusion, Metall. Mater. Trans. A 28A (1997) 10471057.
[6] Y. Iwahashi, Z. Horita, M. Nemoto, T.G. Langdon, The process of grain
refinement in equal-channel angular pressing, Acta Mater. 46 (1998)
33173331.
[7] T.G. Langdon, M. Furukawa, M. Nemoto, Z. Horita, Using equal channel
angular pressing for refining the grain size, JOM 4 (2000) 3033.
[8] V.M. Segal, K.T. Hartwig, R.E. Goforth, In situ composites processed by
simple shear, Mater. Sci. Eng. A 224 (1997) 107115.
[9] L.R. Cornwell, K.T. Hartwig, R.E. Goforth, S.L. Semiatin, The equal channel angular extrusion process for materials processing, Mater. Charact. 37
(1996) 295300.
[10] O.N. Senkov, S.V. Senkova, J.M. Scott, D.B. Miracle, Compaction of
amorphous aluminum alloy powder by direct extrusion and equal channel angular extrusion, Mater. Sci. Eng. A 393 (2005) 1221.
[11] D. Nagarajan, U. Chakkingal, P. Venugopal, Microstructure and mechanical properties resulting from conventional cold extrusion of equal channel
angular extruded aluminium alloy AA 6101, Mater. Sci. Forum 503504
(2006) 287292.

[12] Z. Horita, T. Fujinami, T.G. Langdon, The potential for scaling ECAP:
effect of sample size on grain refinement and mechanical properties, Mater.
Sci. Eng. A 318 (2001) 3441.
[13] D.V. Wilson, P.S. Bate, Influences of cell walls and grain boundaries on
transient responses of an IF steel to changes in strain path, Acta Metall.
Mater. 42 (1994), 1099-1011.
[14] V.M. Segal, Equal channel angular extrusion: from macromechanics to
structure formation, Mater. Sci. Eng. A 271 (1999) 322333.
[15] M. Furukawa, Y. Iwahashi, Z. Horita, M. Nemoto, T.G. Langdon, The
shearing characteristics associated with equal channel angular pressing,
Mater. Sci. Eng. A 257 (1998) 328332.
[16] R.Z. Valiev, T.G. Langdon, Principles of equal channel angular pressing
as a processing tool for grain refinement, Prog. Mater. Sci. 51 (7) (2006)
881982.
[17] J.H. Schmitt, J.V. Fernandes, J.J. Gracio, M.F. Vieiro, Plastic behaviour
of copper during sequential tension tests, Mater. Sci. Eng. A 147 (1991)
143154.
[18] K. Nakashima, Z. Horita, M. Nemoto, T.G. Langdon, Influence of channel angle on the development of ultrafine grains in equal channel angular
pressing, Acta Mater. 46 (1998) 15891599.

You might also like