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Journal of Materials Processing Technology 182 (2007) 363–368

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 This process has been applied to a wide variety of commer-


cially used materials such as aluminium, copper, steel, nickel,
There has been increasing interest in bulk ultrafine grained composites, intermetallics and powder samples [5,8–10]. Exten-
materials as they exhibit superior mechanical properties such sive research has been carried out on the microstructure devel-
as high strength with enhanced ductility, high yield stress and opment and mechanical property evolution during the ECAP
improved toughness [1,2]. An important technique for produc- process. It is well known that ECAP of aluminium alloys leads
ing ultrafine grained materials in bulk form is the equal channel to ultrafine grained structures with improved mechanical proper-
angular pressing (ECAP) [3,4]. In principle, the ECAP die con- ties. However the effects of ECAP on properties and microstruc-
sists of two intersecting channels of equal cross section that ture after subsequent processing by conventional forming oper-
meet at a predetermined angle 2φ (which is usually between 90◦ ations have not been widely investigated. This aspect is impor-
and 135◦ ). The work piece is inserted into the top channel and tant because commercial applications of the ECAP process will
extruded through the bottom channel with the help of a punch. depend heavily on the advantages obtained when it is used as an
The process can be repeated a number of times using the same intermediate forming operation to produce feedstock for subse-
die, because the cross sectional dimensions of the workpiece quent forming by conventional techniques.
do not change before and after processing. By changing the The aim of the present work is to study the applicability of
orientation of the billet between consecutive passes and thereby using ECAP as an intermediate processing step before speci-
changing the strain path of the deformation, different microstruc- mens are processed further through conventional cold extrusion.
tures and mechanical properties can be produced [5–7]. Fig. 1 In effect, the ECAP process was used to produce an ultrafine
shows a schematic diagram of an ECAP die. grained specimen, which was then subjected to conventional
cold extrusion. Previously, improvements in mechanical prop-
erties in a cold extruded AA6101 alloy following ECAP using
∗ Corresponding author. Tel.: +91 44 2257 4775; fax: +91 44 2257 4752. a 120◦ die have been reported [11]. In the current study, the
E-mail address: udaychak@iitm.ac.in (U. Chakkingal). influence of cold extrusion following ECAP of AA 6101 using

0924-0136/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2006.08.016
364 D. Nagarajan et al. / Journal of Materials Processing Technology 182 (2007) 363–368

Table 1
Maximum pressing pressures recorded for different processing routes of ECAP
and ECAP followed by conventional extrusion
Processing route Maximum pressing pressure (MPa)

Pass 1 320
Pass 2A 350
Pass 2C 344
Pass 3A 381
Pass 3C 420
CE of solutionized sample 235
Pass 1 ECAP + CE 287
Pass 2A ECAP + CE 423
Pass 2C ECAP + CE 420

Fig. 1. Schematic diagram illustrating the ECAP process.


3. Results and discussion
a 105◦ die on mechanical properties has been investigated. This
3.1. Pressing pressures
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
An initial peak pressure was observed during the ECAP of this
mechanical properties and microstructure resulting from dif-
alloy for all processing routes except for pass 1 ECAP, where the
ferent processing routes were determined. Comparisons were
extrusion pressure increased continuously with stroke. Table 1
made between properties resulting from specimens directly sub-
summarizes the maximum pressing pressures for different pro-
jected to conventional cold extrusion and specimens subjected to
cessing routes of ECAP and conventional extrusion.
cold extrusion after various ECAP passes. Implications of these
It can be observed that the ECA pressing pressure increased
results on using ECAP as an intermediate processing step prior
from one pass to another for both the processing routes. Pressure
to conventional forming are discussed.
required depends not only on the imposed strain, strain rate, and
2. Experimental procedure temperature of the process, but also on the orientation of micro
shear bands and slip systems with respect to the macroscopic
Aluminium alloy AA 6101 (composition of 0.39% Si, 0.44% Mg, 0.49% Fe, shear planes. Pressing pressure required for route C of ECAP
0.002% Cu, 0.004% Mn, 0.007% Zn, balance Al) was used in this investigation. is higher than route A, which may be due to the changes in
The alloy was solution annealed at 510 ◦ C for 1 h and immediately quenched strain path that increase the interaction between dislocations on
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
intersecting slip planes. This increase in pressure is similar to
angle die (2ϕ = 105◦ ), which imparts 0.88 equivalent plastic strain per pass to the increase in maximum load reported by Horita et al. [12]
the sample, was used for ECAP. The die had a sharp corner, i.e., a corner angle during ECAP of Al alloys 1100 and 3004 for both routes. Higher
of 0◦ . The equivalent plastic strain per pass is given by Segal et al. [3] as pressures were required for the conventional extrusion of pass
2 2A and 2C ECAP subjected specimens.
ε = √ cotϕ
3
where ε is the equivalent plastic strain imparted per pass. 2ϕ is the channel angle 3.2. Hardness
(angle between the two intersecting channels.
Pressing was carried out for three passes using two different processing Table 2 summarizes the hardness values with total strain
routes: route A (no rotation of the sample between consecutive passes) and route
imparted to the sample for various processing routes of ECAP
C (180◦ rotation of the sample about its longitudinal axis between consecutive
passes) with molybdenum disulphide as the lubricant. The extrusion was carried and conventional cold extrusion. In the solutionized condition,
out with an average strain rate of 0.4 s−1 . Specimens have been designated as 2A, the alloy had a hardness of 44 HV2. ECAP through route A
etc. where 2 represents the total number of extrusion passes and A represents the
processing route. Conventional cold extrusion was carried out on solutionized, Table 2
pass 1, 2A and 2C ECAP subjected samples. A conventional extrusion die that Vickers hardness values with total strain (ε) imparted to the sample for various
imparts a strain of 0.78 was selected, which is almost equivalent to the strain processing routes of ECAP and conventional cold extrusion
imparted by the ECAP die in a single pass. Conventional extrusion was carried
Processing route Vickers hardness number
out at an average strain rate of 0.02 s−1 . During extrusion, the force-stroke data
was recorded using a data acquisition system. ε = 0.88 ε = 1.76 ε = 2.64
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 ECAP
processed, and conventionally extruded samples. Ultimate tensile strength and Route A 84 86 95
% elongation to failure were measured. Vickers hardness measurements were Route C 84 100 104
made in both perpendicular and parallel direction to extrusion using a load of Conventional extrusion (CE) 93
2 kg and reported as mean of ten readings. Transmission electron microscopy of solutionized sample
was used to examine the microstructure. Specimens for TEM investigations were Pass 1 ECAP + CE 96
prepared by twin jet electro polishing using a solution of 20% perchloric acid Pass 2 route A ECAP + CE 93
+80% methanol at a temperature of −40 ◦ C. Grain sizes were measured using Pass 2 route C ECAP + CE 98
the linear intercept method.
D. Nagarajan et al. / Journal of Materials Processing Technology 182 (2007) 363–368 365

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 ␧ = 0.88 ␧ = 1.76 ␧ = 2.64

UTS (MPa) % Elongation to failure UTS (MPa) % Elongation to failure UTS (MPa) % Elongation to failure

ECAP
Route A 256 17 307 15 284 14
Route C 256 17 329 16 297 14
Conventional extrusion (CE) 270 19
of solutionized sample
Pass 1 ECAP + CE 345 16
Pass 2 route A ECAP + CE 335 14
Pass 2 route C ECAP + CE 334 14

resulted in hardness of 84, 86 and 95 HV2, respectively, after cessing schedules of ECAP and conventional cold extrusion.
passes 1, 2 and 3. On the other hand, on pressing through route C, Ultimate tensile strength and % elongation to failure of the ini-
the hardness increased substantially to 100 HV2 after 2nd pass tial solutionized material were 99 MPa and 28%, respectively.
of route C and 104 HV2 after the third pass. This is because the When this solutionized material was subjected to ECAP, UTS
rotation of the specimen by 180◦ between consecutive passes increased remarkably up to two passes for both the processing
increases the dislocation interactions on intersecting slip planes routes; 99 MPa to 307 MPa for route A and 99–329 MPa for
[11]. route C. The % elongation to failure decreased from 28 to 15%
Hardness value of 93 was observed after conventional cold for route A and 16% for route C. Strength decreased after the
extrusion of solutionized specimens. Conventional cold extru- third pass for both the processing routes A (307 MPa after second
sion carried out on passes 1 and 2A ECAP subjected specimens pass to 284 MPa after third pass) and C (329 MPa after second
resulted in slight increase in the hardness. Hardness remained pass to 297 MPa after third pass) of ECAP. This is due to the
nearly the same after conventional extrusion of pass 2C ECAP disruption and dissolution of the original dislocation cell struc-
subjected specimens. ture, which leads to a reduction in work hardening [13]. This
results in the decrease in the volume fraction of cell structures
3.3. Tensile strength and elongation at fracture and dislocation density, which cause an increase in the mean free
path of dislocations. This trend is in line with previous results
Table 3 summarizes the values of ultimate tensile strength obtained during ECAP with a 120◦ die [11]. This is also sup-
and % elongation to failure with total strain for various pro- ported 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) 363–368

(microstructure after pass 2 route A) and Fig. 2(d) (microstruc- [16]. Because there is a change in strain path, there may be an
ture after pass 2 route C) show a clear dislocation cell structure initial shortage of mobile dislocations in newly activated slip
which was reinforced during the new deformation mode. How- systems and this can result in an increase in strength [17]. This
ever, Fig. 2(e) (microstructure after pass 3 route A) and Fig. 2(f) is also supported by the fact that extrusion pressures for pro-
(microstructure after pass 3 route C) show a partially dissoluted cessing by route C are consistently higher than that for route
dislocation cell structure with an apparent lower dislocation den- A.
sity. The % elongation to failure decreased from 16% to 14% Conventional extrusion carried out on solutionized specimens
after 3rd pass for both the processing routes. resulted in UTS of 270 MPa and % elongation to failure of 19%.
Processing by route C gave higher mechanical properties as Conventional cold extrusion of passes 1, 2A and 2C ECAP pro-
compared to processing by route A. This is in contrast to most cessed specimens showed increase in strength compared to prior
of the previous work in which processing by route A resulted in ECAP deformed condition, due to the continuous reinforcement
higher strengths [5,12,14]. However, it should be noted that all of dislocation cell structure that was created in the previous
these previous investigations used a die angle, 2ϕ = 90◦ . Such deformation step. At an identical level of strain, the % elonga-
an angle leads to reversal of shear during successive passes by tion to failure is the same for materials processed through ECAP
route C along the macroscopic plane of shear. This leads to dis- and ECAP followed by conventional extrusion. This implies that
location annihilation and somewhat lower strengths after route the processing route does not have a significant influence on
C processing compared to processing by route A. However, the the % elongation to failure of the material. Highest strength of
current study was carried out using a die angle of 105◦ . There- 345 MPa was obtained for specimens subjected to pass 1 ECAP
fore, strain reversal during successive passes by route C does not followed by conventional cold extrusion.
occur. On the other hand, the macroscopic shear planes intersect
each other at a finite angle for a 105◦ die. Therefore for die angles 3.4. Microstructural characteristics
greater than 90◦ , route C processing can lead to higher strengths.
The shearing characteristics and the macroscopic shear planes Fig. 2 shows the TEM micrographs of the ECAP sub-
involved during ECAP and their variation with processing routes jected samples processed through various routes. The grain size
have been investigated by Furukawa et al. [15] and Valiev et al. 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) 363–368 367

After first pass, the grain size was reduced to 0.58 ␮m and well known that imparting higher strain per pass (through use
it consisted mainly of parallel bands of elongated subgrains of die angles closer to 90◦ ) is more conducive to the production
(Fig. 2(b)). After second pass, the grain sizes were approxi- of an ultrafine grained microstructure with a large proportion of
mately 0.5 ␮m for both processing routes (Fig. 2(c) and (d), high angle grain boundaries [16,18]. In addition, the choice of
respectively). After third pass, the grain sizes were about the die angle also determines the strain path and the extent of strain
same (Fig. 2(e) and (f), respectively), but dissoluted disloca- reversal between successive passes for the various processing
tion cell structure with lower dislocation density was observed. routes. It can be expected that different results may be obtained
This is also reflected in mechanical properties in the form of a if ECAP is carried out using a 90◦ die before cold extrusion.
decrease in tensile strength from second to third pass for both This has certain implications with regard to commercializa-
the processing routes. Relative misorientations between adjacent tion of ECAP. If ECAP is used as an intermediate processing
grains/subgrains were not measured in this study. step to produce feedstock material which is to be later pro-
Conventional extrusion carried out on solutionized samples cessed by conventional forming techniques like forging, extru-
showed an average grain size of 0.59 ␮m. There was no further sion, drawing, etc., high levels of severe plastic deformation
grain refinement observed during cold extrusion of passes 1, 2A (SPD) strains may not always translate into a product with opti-
and 2C ECAP processed specimens. Though aluminium and its mum mechanical properties. Levels of optimum SPD strain to
alloys undergo grain refinement initially with increasing defor- be imparted to the feedstock may have to be decided based on
mation, these values normally stabilize in the submicron range the ECAP die angle used and the subsequent processing route to
with further deformation not leading to grain refinement. Typi- be employed. The SPD microstructure obtained by ECAP can
cal microstructures after ECAP followed by cold extrusion are therefore be regarded as inherently unstable and susceptible to
shown in Fig. 3. flow softening depending on strain paths encountered in further
processing.
3.5. ECAP as a deformation step prior to conventional cold
extrusion—enhancement in mechanical properties 4. Conclusions

When ECAP is used an intermediate processing step to pro- Intermediate processing by ECAP to one pass followed by
duce specimens for subsequent cold extrusion, it is observed conventional extrusion leads to enhanced mechanical properties
from Table 3 that increases in mechanical properties are obtained in the extruded specimens with only a small reduction in duc-
with only a slight decrease in % elongation at failure. Conven- tility. Conventional cold extrusion after ECAP did not result in
tional cold extrusion of a solutionized specimen resulted in an further grain refinement. ECAP can effectively be used as an
UTS of 270 MPa, hardness of 93 HV2 and elongation at frac- intermediate processing step prior to conventional cold extru-
ture of 19%. However after cold extrusion using a specimen that sion for property enhancement in the cold extruded Al alloy
had been subjected to one pass of ECAP, the strength increased AA6101. Additional plastic deformation through two passes to
to 345 MPa, hardness increased to 96 HV2 while elongation at produce a stronger material did not result in any benefit as far as
fracture decreased only slightly to 16%. The fine grains resulting the cold extruded product mechanical properties are concerned.
from ECAP helped to maintain a good ductility even after sig- High levels of SPD strain imparted to the specimen or feedstock
nificant straining from cold extrusion. This implies that ECAP may not always yield optimum mechanical properties after sub-
can be used as a prior deformation step to conventional extrusion sequent forming operations. Therefore optimum levels of SPD
for property enhancement in the cold extruded AA6101 alloy. strain may have to be decided based on the ECAP die angle used
However what is significant is that subjecting the speci- and subsequent forming techniques to be employed.
mens initially to two passes of ECAP prior to cold extrusion
did not result in further improvements in mechanical proper-
Acknowledgements
ties of the cold extruded specimen. On the contrary, as shown
in Table 3, processing through two passes by ECAP followed
This work was carried out as part of a research project spon-
by cold extrusion resulted in lower mechanical properties of the
sored by Department of Science and Technology, Government
extruded product (lower UTS of 335 MPa and lower % elon-
of India and this assistance is gratefully acknowledged.
gation of 14% at failure) compared to specimens subjected to
only one pass of ECAP prior to cold extrusion. This implies that
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