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around its
longitudinal axis before each consequent pass [16,19,20,22]. Direct
experimental investigations of the effect of strain reversal at large
strains onstructureandmechanical properties evolutionweredone
for pure Ni and Armco Fe [23], AlMgSc alloy [24], pure Ti and
low carbon steel [25]. This effect was also discussed in theoretical
works [26,27]. In these reports, it was found that the strain reversal
has signicant effect on the structure evolution, but it is signif-
icantly different depending on material, and hence other direct
experimental investigations of this effect is of great interest.
Therefore, the present research was aimed to clarify the effect
of strain reversal on grain renement in pure aluminum in direct
experiments. For this purpose, HPT technique was utilized. Among
other SPD techniques, only HPT allows to introduce precisely con-
trolledvalues of simple shear strainas well as directionof straining,
and therefore is the most appropriate for the present research.
2. Experimental
In this study aluminum of 99.99% purity was used. The as-
received cold rolled sheet of 1mm thickness was cut into 10mm
in diameter samples. The samples were mechanically grinded to
0.6mm thickness, annealed for 1h at 500
rotation in clock-
wise direction followed by counterclockwise rotation up to the
same degree. So that one cycle of 12
clockwise followed by 12
rotation
in one direction. Four cycles of the reversal deformation is equal
to 96
12
1 0 1.01 2.02
96
12
4 0 4.03 8.06
the case if 60
3
r
h
(1)
where is equivalent strain, r is a specimen radius, h is a specimen
thickness, and is a torsion angle in radians. Numerical values of
accumulated strains used in this study are shown in Table 1.
The structure characterization was carried out on the mid-
section perpendicular to axial direction of the as-processed
specimens by using transmission electron microscopy (TEM) and
electron backscattered diffraction (EBSD) techniques in a scanning
electron microscope equipped with a eld-emission type electron
gun (FE-SEM). Thin foils for TEMwere prepared by cutting samples
of 2mm3mmusing a diamond cutter, grinding themon sandpa-
per to thickness of 0.1mm and nally twin-jet electro-polishing
in a 30%HNO
3
+70%CH
3
OH solution at 20
C to perforation. The
TEM observations were done in Hitachi H-800 operated at 200kV.
For EBSDanalysis, specimens were grinded on sand paper, polished
with alumina powder suspensions and nally electro-polished in
a 30%HNO
3
+70%CH
3
OHsolution at 20
. The micrographs a and d, b and e, c and f were obtained at specimens axis, middle radius and edge, respectively.
D. Orlov et al. / Materials Science and Engineering A 499 (2009) 427433 429
Fig. 3. TEMmicrographs of the 99.99%Al after HPT processing. The micrographs a, b and c correspond to monotonic straining to 96
. The micrographs a and d, b and e, c and f were obtained at specimens axis, middle radius and edge, respectively.
grain renement through grain subdivision are clearly seen from
these gures. Detailed analysis of mechanisms of the microstruc-
ture evolution in pure aluminum under SPD is rather well done in
the previous references [2832]. Mechanisms of the microstructure
evolution observed in this study are quite consistent with the pre-
vious knowledge. However, there are some particular differences in
structural evolution between monotonic and reversal deformation
modes.
Comparing the micrographs in Fig. 2, one can see that after the
torsion equivalent to 24
rotation; d, e and f
correspond to 1 cycle of reversal straining with amplitude of 12
. The maps a and d, b and e, c and f were obtained at specimens axis, middle radius and edge, respectively.
Boundaries with angles of misorientation 2
<15
are shown in grey lines, while boundaries with misorientations larger than 15
are in black.
430 D. Orlov et al. / Materials Science and Engineering A 499 (2009) 427433
Fig. 5. Boundary maps obtained from EBSD analysis of the 99.99%Al after HPT processing. The maps a, b and c correspond to monotonic straining to 96
rotation; d, e and f
correspond to 4 cycles of reversal straining with amplitude of 12
. The maps a and d, b and e, c and f were obtained at specimens axis, middle radius and edge, respectively.
Boundaries with angles of misorientation 2
<15
are shown in grey lines, while boundaries with misorientations larger than 15
are in black.
as was shown in Table 1. At the specimens edge ( 2, Table 1) in
the case of monotonic straining, most of subgrains are almost free
of dislocations, and the (sub)grain boundaries are quite thin and
straight. In case of the reversal straining, there are still arrays of
dislocations within the subgrains and in vicinity of the (sub)grain
boundaries even at the specimen edge. In the areas of the middle
radius, transition between the structures on axis and edge is seen.
This conrms the gradual evolution of the ultrane grained struc-
tures during severe plastic deformation; i.e., dislocation activation,
accumulation, rearrangement and nally (sub)grain boundary for-
mation leading to the ultrane grains. It was also found that in
the case of reversal deformation this microstructural evolution is
retarded in comparison with monotonic one.
Fig. 3 shows that after the torsion equivalent to 96
rotation
(maximum strain 8, Table 1), the structure inhomogeneity in
the specimens cross-sections is still kept for both modes of defor-
mation. On the specimen axis, almost no change in the structure
could be seen, compared with Fig. 2(d), in the case of the rever-
sal deformation; while in the case of the monotonic deformation
reduction in dislocation density and formation of limited num-
ber of subgrain boundaries are apparent. At the specimens edge
the (sub)grains are free of dislocations, reasonably equiaxed and
Fig. 6. Microstructural parameters obtained from the EBSD data showing the structure evolution with strain accumulation in the 99.99%Al HPT processed. Subgrain sizes
development at edge part of the specimens (a) and fraction of grains surrounded by HABs (the boundaries with misorientations 15
as well
as the peak at very low angle. The reversal deformation to the
same equivalent strain does not lead to the second peak forma-
tion.
Subgrain boundaries having very low misorientation smaller
than 2