Materials Transactions, Vol. 50, No. 1 (2009) pp.

87 to 91
Special Issue on Severe Plastic Deformation for Production of Ultrafine Structures and Unusual Mechanical Properties: Understanding Mechanisms
#2009 The Japan Institute of Metals

Grain Refinement and Mechanical Behavior of the Al Alloy,

Subjected to the New SPD Technique
Ruslan Z. Valiev* , Maxim Yu. Murashkin, Elena V. Bobruk and Georgy I. Raab
Institute of Physics of Advanced Materials, Ufa State Aviation Technical University, 12 K.Marx str., Ufa 450000, Russia

The paper focuses on producing of ultrafine-grained (UFG) structure in the Al 6061 alloy by a new severe plastic deformation (SPD)
technique, developed recently in our laboratory, namely equal channel angular pressing with parallel channels (ECAP-PC). The evolution of
microstructure at ECAP-PC was examined and was proved that the alloy becomes of a homogenous UFG structure after 4 passes. Such a
structure increases essentially the alloy’s mechanical properties, specifically strength and ductility. The advantages of this new technique in
producing of UFG alloys over conventional ECAP are considered and discussed as well. [doi:10.2320/matertrans.MD200821]

(Received August 18, 2008; Accepted October 27, 2008; Published December 25, 2008)
Keywords: ultrafine-grained structure, severe plastic deformation, equal channel angular pressing with parallel channels, strength and
ductility

1. Introduction used in a cast condition. The alloy under investigation was

characterized by lower level of alloying elements (Si and
Fabrication of ultrafine-grained (UFG) metals and alloys Mg), comparing to traditional Al 6061 alloy.8) Before
by severe plastic deformation (SPD) processing has become a ECAP-PC treatment, initial billets were subjected to solid
well-known direction in modern materials science.1–3) These solution treatment for 5 h at 530
C with the following water
works started in the early 90-s with two techniques: equal quenching.
channel angular pressing (ECAP) and high pressure torsion The principles of ECAP with PC are shown in Fig. 1.5,7) A
(HPT),4) have been developed intensively last decade in distinctive feature of the ECAP-PC is that during a single
connection with creation of principles of materials nano- processing pass, two distinct shearing events take place:
structuring for advanced properties and elaboration of more shear in two deformation zones subsequently corresponding
effective SPD techniques. to two subsequent channels intersections in the die-set
Conventional ECAP technique, widely used to produce (Fig. 1(a), (b)).
UFG structure in metals and alloys is currently applied The value of the displacement between the two channels,
mainly as laboratory-based SPD method as it has some K, and the angle of intersection of the two channels
, are the
limitations, which restrict its industrial application. These main parameters of the die geometry, which influence both
restrictions are due to labor-intensity and low efficiency of the flow pattern and the strain-stress state of the ECAP
the method, because a large number (8–12) of passes is process. It has been established by computer simulation, that
required for a UFG structure formation and only small the optimal value of these parameters leading to the largest
amount (less than 60%) of the material is subjected to strain homogeneity are
¼ 100
and K ¼ d, where d is the
homogenous shear straining in the bullet.5) The new SPD channel diameter.5,7) Under these conditions, the accumulate
technique-equal channel angular pressing with parallel strain for one pass is approximately equal to 2. The
channels (ECAP-PC),6,7) newly developed in our laboratory simulation results have been confirmed experimentally using
is able to reduce a number of restrictions for the conventional a grid method. Furthermore, the studies showed that the
ECAP. Computer simulation and experiments applied to Cu deformation pattern realized in ECAP-PC die-set optimal
and Ti as model materials have shown, that UFG structure geometry makes the structure homogeneous along the length
is produced more effectively by ECAP-PC, due to more of the bulk sample including up to the ends (the material
advanced strain and homogeneity rates.5,7) utilization ratio is higher than 90%).
The given paper reports the first successful application of Billets of 6061 Al alloy with the diameter of 18 mm and
the new SPD technique to commercial Al alloy with the aim 100 mm length were subjected to ECAP-PC at 100
C, since
of producing an UFG structure and improving its mechanical the temperature provides significant grain refinement, pre-
properties. The experiment was conducted on 6061 Al alloy. serving the facility for its further strengthening by subsequent
This alloy is one of the commercial aluminum alloys widely aging at 160–175
C.
used in aerospace and automobile industries. Advantages Vickers hardness (HV) was measured using a Micromet-
of the new method versus conventional ECAP are being 5101 microidentation tester with a load of 200 g for 15 s. In
discussed as well. order to receive reliable results, each sample was measured
more than 10 times.
2. Experimental Procedure Tensile tests at room temperature were performed on
Instron 1185 at a strain rate of 5  104 s1 . Mechanical
A commercial 6061 aluminum alloy (0.80Mg-0.41Si- properties were measured by at least 2 specimens with gage
0.12Cu-0.03Mn-0.02Ti-0.22Fe-balance Al (mass%)) was length 15 mm and diameter of 3 mm. Tensile specimens were
cut of parallel to the longitudinal axis of the ECAP-processed
*Corresponding author, E-mail: [email protected] material.
88 R. Z. Valiev, M. Yu. Murashkin, E. V. Bobruk and G. I. Raab

a b c

Fig. 1 The principles of ECAP with parallel channels: (a) a view of the deformation zone obtained by two dimensional finite element
method (2-D FEM). (b) a schematic illustration where N is in the shear direction; d-diameter of the channel; K- is the displacement
between the two channels;
- is the angle of intersection between the two parts of the channel and the internal shaded areas depict the
sharing as the sample traverses the shearing zone; (c) a general view of the experimental ECAP die-set.

a b

Fig. 2 Microstructure of Al 6061 alloy after ECAP-PC through one pass: dark field (a), SAED pattern (b).

The structural characterization by TEM was performed in grains of 500 nm are also observed in the structure along with
JEM-100B and JEOL-2000 EX electron microscopes using subgrain fragmentation (Fig. 3(c), (d)).
dark and bright fields. Average grain size was estimated from The electron diffraction pattern (Fig. 3(f)) represents
more than 250 grains measurement. numerous spots distributed uniformly over the circles. This
testifies to formation of the UFG structure at the areas of a
3. Results and Discussion granular type with high-angle grain boundaries at the areas.
The UFG structure formed after ECAP-PC through 4
Observations by TEM showed that mainly subgrain passes is also of equiaxed (Fig. 4). Besides, secondary phase
structure of a lamellar type with clear orientation to shear dispersive precipitates of less than 10 nm in size were found
plane was formed after ECAP-PC thorough one pass at in the alloy UFG structure after ECAP-PC (Fig. 4, A and B
100
C (Fig. 2(a)). The mean cross subgrain size comprised areas). According to the results9,10) dealing with 6061 Al
400 nm and longitudinal one made up 1200 nm correspond- alloy processing by conventional ECAP, these dispersive
ingly. Electron diffraction patterns prove subgrain structure precipitates represent Mg2 Si particles. These precipitates
formation with mainly low-angle grain boundary misorien- testify to the UFG structure formation being accompanied by
taions (Fig. 2(b)). After ECAP-PC through the second pass at dynamic aging at ECAP-PC through 4 passes. As the
the same temperature the structure changed significantly. precipitates were not found after the ECAP-PC through 1
(Fig. 3). Fragmentation by means of cross-subboundary and 2 passes, we can suggest that they are absent in these
formation can be seen in elongated subgrains formed after states, or their size was quite small and required investiga-
ECAP-PC through 1 pass (Fig. 3(a), (b)). Separate areas tions by high-resolution electron microscopy. It should be
(with a volume fraction of around  30%) of equi-axed also noted that there were more lattice dislocations in the
 Grain Refinement and Mechanical Behavior of the Al Alloy, Subjected to the New SPD Technique 89

a c

A’

d e f

Fig. 3 Microstructure of the alloy after ECAP-PC through 2 passes: subgrain fragmentation (a), (b), grain structure (d), (e)-bright and dark
fields) SAED patterns (c), (f).

structure after 1 and/or 2 passes (Fig. 2 and 3) when At the same time the homogeneous UFG structure (Fig. 4)
compared to the structure formed in the material after 4 formed after ECAP-PC through 4 passes leads to insignificant
passes (Fig. 4). loss in strength. However, its ductility increases by two times
The Vickers hardness (HV) of the initial billets after solid and its elongation reaches  20%. Herewith, the UFG alloy
solution treatment was 410  18 MPa. ECAP-PC processing demonstrates considerable uniform elongation which makes
increases the rates up to 1155  24 MPa and to 1220  up  9%. Such a high value, which comprises  40{45%
27 MPa after 1 and 2 passes correspondingly. However, the from total elongation, shows that the alloy with UFG
hardness values decreased to 1100  21 MPa after ECAP-PC structure has a potential to display enhanced fatigue.5,11)
through 4 passes. Mechanical properties of 6061 alloy after Thus, the analysis of structural changes in the alloy 6061
ECAP-PC through 1, 2 and 4 passes are presented in Fig. 5 after ECAP-PC at 100
C proves that the ECAP-PC technique
and Table 1. The data can be compared with that of the same makes it possible to produce a homogeneous UFG structure
alloy after conventional T6 treatment (quenching at 535
C in a cast alloy after 4 passes in comparison with 8–10 passes
and subsequent artificial aging at 160
C for 12 hours). in conventional ECAP,5,9) in other words, using of ECAP-PC
The results correlate closely to the evolution of the can decrease the number of passes in 2–3 times under nearly
microstructure revealed (Fig. 2–4). The formed substructure the same processing conditions. Another advantage of the
(Fig. 2) with a high density of lattice dislocations provides pressing is significant increase in the volume of UFG
significant increase in strength after ECAP-PC through 1 structure in a billet processed: about 85–90% compared to
pass, but its ductility is low enough and elongation to failure 50–60% after conventional ECAP. This can be of special
comprised  6:5%. The formation of the UFG structure of a interest for the process industrial application.
combined type containing grains and subgrains (Fig. 3) in Regarding UFG structure formation in the alloy, an
the billets after ECAP-PC through 2 passes provides some important feature of ECAP-PC is producing of practically
increase in both strength and ductility up to  8% (Table 1). equiaxed UFG structure already after 2 passes (Fig. 3),
90 R. Z. Valiev, M. Yu. Murashkin, E. V. Bobruk and G. I. Raab

a b c

A 100 nm B 100 nm

Fig. 4 Microstructure of the alloy after ECAP-PC through 4 passes in the longitudinal section of the sample (a), (b), in the cross-section of
the sample (disperse particles of Mg2 Si phase precipitated during the processing-areas A and B) (d), SAED pattern (c).

Table 1 Mechanical properties of the 6061 Al alloy at room temperature

after ECAP-PC at 100
C.

UTS, YS, El.,

500 Treatment
(MPa) (MPa) (%)
Engineering Stress (MPa)

1 pass
2 passes ECAP-PC at 100
C, 1 pass 370 335 6.5
400
4 passes ECAP-PC at 100
C, 2 passes 380 350 8.0


ECAP-PC at 100 C, 4 passes 345 305 20.0
300 T6 T6 230 178 30.0

200
though the grains observed after the first pass were of
100 elongated laminar structure (Fig. 2(a)). Gradual transforma-
after ECAP in PC at 100°C
tion of the grains to equiaxed ones is typical also of
conventional ECAP.5) At the same time, the present work
0
0 5 10 15 20 25 30 35 40 proves the connection of this transformation with the
formation of low-angle subgrain boundaries inside the
Engineering Strain (%) elongated grains (Fig. 3(a)) and their following arrangement
Fig. 5 The engineering stress-strain curves of the 6061 Al alloy at room to high angle boundaries of the equiaxed UFG structure.
temperature after ECAP-PC processing and convention heat-treatment Similar evolution of nanostructure during SPD processing
(T6). has been discussed elsewhere.12)
 Grain Refinement and Mechanical Behavior of the Al Alloy, Subjected to the New SPD Technique 91

One more effect revealed in the alloy after 4 passes is the (3) The 6061 Al alloy after ECAP-PC through 4 passes
formation of highly-disperse precipitations of the second showed combination of high strength and ductility,
phase, obviously, the particle of Mg2 Si phase. The formation which is of special interest for its advanced application.
of such particles evidences dynamic aging, which was
observed recently in 6061 alloy after conventional ECAP.9,10) Acknowledgements
However, this time the aging occurs at a low temperature
(100
C) and aging time less than 10 minutes, which is The present paper was supported in part through grants of
considerably lower, than 175
C, 8 h of the peak aging the Ministry for Education and Science of the Russian
condition (T6) for a 6061 alloy.9) Such an acceleration of Federation and Russian Foundation for Basic Research as
aging kinetics can result from high vacancy concentration well as by the NIS-IPP Program of DOE (USA). Cooperation
during processing. Recent ‘‘in situ’’ HPT experiments in with co-authors mentioned in references is gratefully ac-
synchrotron beamline showed13) that excess vacancy con- knowledged as well.
centration can reach 105 , which is near to equilibrium
concentration at melting temperature point. Besides, 3D atom
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