Materials Science and Engineering A 499 (2009) 427433

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Materials Science and Engineering A
j our nal homepage: www. el sevi er . com/ l ocat e/ msea
Role of strain reversal in grain renement by severe plastic deformation
Dmitry Orlov
a,
, Yoshikazu Todaka
b
, Minoru Umemoto
b
, Nobuhiro Tsuji
a
a
Department of Adaptive Machine Systems, Graduate School of Engineering, Osaka University, 2-1 Yamada-oka, Suita, Osaka 565-0871, Japan
b
Department of Production Systems Engineering, Toyohashi University of Technology, Tempaku-cho, Toyohashi, Aichi 441-8580, Japan
a r t i c l e i n f o
Article history:
Received 13 June 2008
Received in revised form 26 August 2008
Accepted 5 September 2008
Keywords:
Strain reversal
Aluminum
HPT
EBSD
TEM
Grain subdivision
a b s t r a c t
Most of severe plastic deformation processes involve strain reversal. Till now quite big number of
researches has been done on indirect study of its role, which discusses the effect of loading path in
ultra-ne grained structure formation. This work is aimed to study directly the role of the strain rever-
sal in grain renement by severe plastic deformation. A 99.99% purity aluminum was processed by high
pressure torsion up to 96

rotation (maximal equivalent strain 8) with two deformation modes: mono-

tonic and reversal deformations with a step of 12

rotation (maximal equivalent strain 1). It was shown

that strain reversal retarded the grain renement in comparison with the monotonic deformation. This
explains slower rate of the nanostructure formation of the SPD processes that involve strain reversal.
2008 Elsevier B.V. All rights reserved.
1. Introduction
At the present time, severe plastic deformation (SPD) is a well
proved tool for fabricating ultrane-, nano- [13] and even amor-
phous [4,5] structures in metallic materials. Under SPD processing,
a desired structure is formed continuously fromtop coarse grains
down to ultra-ne/nano-grains or amorphous. There are several
SPD methods developed during last two decades. Most of them
involve reversal straining essentially, e.g. repetitive corrugation
and straightening [6], cyclic extrusion and compression (CEC) [7],
twist extrusion (TE) [8], and multidirectional forging (MF) [9,10],
whileother techniques, e.g. accumulativeroll bonding(ARB) [11,12],
applies (quasi)monotonic straining. In some processes, deforma-
tion path might be varied depending on need, e.g. high pressure
torsion (HPT) [13] and equal channel angular extrusion (ECAE)
[14]. However, effects of loading scheme and deformation path on
structure development, especially in case of ECAE [1521], are still
discussed vigorously.
Effects of accumulated strain value, deformation temperature,
strain rate and hydrostatic pressure on microstructure evolution
have been studied already rather well, while the effect of strain
reversal under large strainaccumulationis studiedstill moderately.
The role of strain reversal in ow stress drop (Bauschinger effect)
and structure evolution has been studied well enough for fatigue

Corresponding author. Tel.: +81 668794173; fax: +81 668794174.

E-mail address: orlov@ams.eng.osaka-u.ac.jp (D. Orlov).
test conditions. But in the fatigue tests, plastic strain introduced is
up to 1%. For the case of severe plastic straining, the strain rever-
sal has been studied marginally for the case of ECAE processing
by route C that involves rotation of a specimen by 180

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

C and cooled in a fur-

nace. As a result, initial material had fully recrystallized structure
with an average grain size of 290m.
0921-5093/$ see front matter 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2008.09.036
428 D. Orlov et al. / Materials Science and Engineering A 499 (2009) 427433
Fig. 1. Schemes of HPT processing routes used in this study. The diagraminserted in
the gure shows the principal difference between monotonic and reversal straining.
CW and CCW mean clockwise and counterclockwise rotations, respectively.
HPT processing was done continuously, without stops between
torsion direction changes, according to the schemes shown in Fig. 1
at room temperature and speed of 0.22 rotation per minute. Tor-
sions up to 96

were used for the case of monotonic loading. For

reversal straining, samples were deformed to 12

rotation in clock-
wise direction followed by counterclockwise rotation up to the
same degree. So that one cycle of 12

clockwise followed by 12

counterclockwise rotations is mathematically equal to 24

rotation
in one direction. Four cycles of the reversal deformation is equal
to 96

of monotonic counterpart. The processing was continuous

for the both deformation modes, and the processing time intervals
were equal. This increment in the step size (12

rotation) under the

HPT processing was chosen since within the specied tool geom-
etry, it was comparable with the strain for 1 pass of ECAE (in the
case if 90

of channels intersection die is used) or 1 pass of TE (in

Table 1
Equivalent strain values achieved in this study (estimated by Eq. (1)).
Torsion angle Position in the specimen
Monotonic Reversal Axis Middle of radius Edge
24

12

1 0 1.01 2.02
96

12

4 0 4.03 8.06
the case if 60

of twist line slope angle die is used) or 2 passes of

ARB.
Strain values under the HPT processing were estimated by the
following equation [2]:
=
1

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

C. The observations were

done in FEI Sirion FE-SEM facility equipped with TSL orientation
imaging microscopy system. For all statistical analysis from the
EBSD data, at least 1500 (sub)grains were considered.
3. Results
Micrographs resulting from the TEM observations are shown
in Figs. 2 and 3. Development of dislocation substructures and
Fig. 2. TEM micrographs of the 99.99%Al after HPT processing. The micrographs a, b and c correspond to monotonic straining to 24

rotation; d, e and f correspond to 1 cycle

of reversal straining with amplitude of 12

. 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

rotation; d, e and f correspond to 4 cycles

of reversal straining with amplitude of 12

. 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 for both monotonic and rever-

sal modes, the structures are inhomogeneous in the specimens
cross-sections. In the areas close to the specimens axis, disloca-
tion substructures typical for early stages of grain renement in
severe plastic deformation are seen. The microstructures also indi-
cate that plastic deformation certainly occurred to some extents,
though the strain value on the specimen axis is ideally zero in HPT,
Fig. 4. 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 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

) in total number of subgrains (the

strain-inducedcells surroundedby boundaries withmisorientations 2

, the minimumangular misorientationresolutiondetectable by the EBSDtechnique) (b). The statistics

was calculated from at least 1500 (sub)grains.
D. Orlov et al. / Materials Science and Engineering A 499 (2009) 427433 431
Fig. 7. Misorientation angle proles obtained fromEBSDanalysis of the 99.99%Al HPT processed. Positions where the EBSDmaps were obtained are shown in the illustrations
inserted in the diagrams schematically. The maps a, b and c correspond to monotonic straining; d, e and f correspond to reversal straining.
surrounded by sharp boundaries in the both cases of deformation
modes. Themiddleradius areas showsignicant differenceinstruc-
ture: well dened (sub)grains but still containing dislocations in
the case of reversal deformation, while clear grains surrounded by
sharp boundaries and free from dislocations inside in the mono-
tonic specimen. These observations suggest rather sharp change in
the microstructure depending on the distance fromthe specimens
axis, i.e., strain.
According to the EBSD observations, initial structure was sig-
nicantly rened by the HPT processing, as can be seen from the
boundary maps shown in Figs. 4 and 5. The structure inhomo-
geneity depending on the distance from the specimens centers
discovered in TEM observations is well conrmed in larger views
by the EBSD analysis. The inhomogeneity is less in monotonic
deformation and decreases with increasing total accumulated
strain value (rotation degree/number of cycles). Depending on the
distance from the specimens axis, continuous evolution of struc-
ture from subgrains with low angle boundaries (LABs), through
rather heterogeneous mixtures of high angle boundaries (HABs)
intersected by LABs, to ultrane-grained equiaxed structure with
dominating HABs at the specimens edge could be seen for both
monotonic and reversal specimens.
The average (sub)grain sizes obtained from the EBSD data are
summarized in Fig. 6. For all the data shown there, statistics was
calculated fromat least 1500 (sub)grains. For the both deformation
modes, very ne subgrain size of about 1.01.2m was achieved
at the specimens edge already after the torsion equivalent to
24

rotation (equivalent strain 2, Table 1). Further processing

affects the average subgrain size very slightly, but number of the
grains surrounded by HABs increases. This effect is very much pro-
nounced in the case of monotonic deformation, but much slower
for the reversal counterpart. The boundary misorientation pro-
les shown in Fig. 7 are in good agreement with the qualitative
results from the TEM observations and also suggest the retarda-
tion in the structure evolution in reversal deformation. On the
specimens axis (Fig. 7a and d), there is a distribution of misori-
entation angles with a strong peak in LABs region for the both
deformation modes. Almost no change in the misorientation dis-
tribution is seen with increasing strain in the case of reversal
deformation, while monotonic deformation leads to the increase
of HAB fraction. In the areas of the specimens middle radius and
edge for the 96

rotated samples, distributions of the misorien-

tation angles are bimodal with small peak around 45

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

and therefore out of the EBSDresolution, do not affect prin-

cipally the results shown above. Taking them into account would
slightly decrease the average subgrain sizes and average angle of
misorientations, but would not affect qualitatively the conclusions
concerning the effect of strain reversal on structure development
under large plastic straining. Slight discrepancy in the EBSD and
TEM observations for the middle radius area for the deformations
equivalent to 96

rotation, might be attributed to local effect owing

to the structure inhomogeneity.
4. Discussion
The structure inhomogeneity along specimens radius at early
stages of the processing reported in the previous section corre-
sponds to the strain gradient introduced during the processing.
Such a structure inhomogeneity is not surprising but a well known
feature in the HPT processing under monotonic straining con-
ditions, and usually the structure homogeneity is achieved by
excessive torsion. At the same time, the absence of ultrane grained
structure evolution in vicinity of the specimens axis (where strain
amplitude is smallest) and the increase in the structure inhomo-
geneity with increasing strain are specic features of the reversal
straining by HPT.
432 D. Orlov et al. / Materials Science and Engineering A 499 (2009) 427433
Such behavior of the structure evolution is thought to be a con-
sequence of a kind of the Bauschinger effect. It is interesting to nd
that the Bauschinger effect works not only in near elastic deforma-
tion, but also even in the far plastic region of deformation. And due
to this effect, formation of HABs in the case of reversal straining is
signicantly retarded in comparison with monotonic counterpart.
Based on the conclusions from the article by Hasegawa et al.
[33], in addition to the reversed motion of free isolated disloca-
tions within cells or subgrains, cell walls and sub-boundaries are
also unstable against strain reversal. For low strain values, the
decrease in dislocation density about 16% at early stages of reversal
deformation was reported. These results are very well consistent
qualitatively with the results of the present work.
When present results are compared with earlier reports, it
could be seen that behavior of pure Al is quite different from pure
Ti [25]: while strain reversal retards formation of HABs in alu-
minum, in titaniumit results in faster formation of equiaxed grains
surrounded by HABs. This difference should be attributed to the
difference in lattices of these materials (face-centered cubic lattice
in Al, and hexagonal close-packed in Ti). At the same time, materi-
als with similar cubic lattices (Ni and Fe) studied in [23], showvery
similar behavior to our results: fractions of HABs in the deformed
structures were highest in the monotonic deformation mode, and
lower after the reversal deformation. In [23], minimal grain sizes
reached after high strains were also affected by the deformation
mode: after reversal deformation average grain sizes were larger
than after the monotonic counterpart. In our research, at the spec-
imens edge, where the strain amplitude was the largest, after the
reversal deformation, the average grain size was 0.1m larger
than that after the monotonic one. This difference is much less than
the deviations in the grain size distributions (Fig. 6) and could be
considered as negligibly small. However, the reversal deformation
withvery lowstrainamplitude invicinity of the specimens axis did
not lead to ultra-ne grains formation at all. So that our results on
pure Al are very consistent with results of other researches on pure
Ni and Armco Fe. Nevertheless, more detailed, study of the effect of
amplitude of strain reversal should be done to further clarify this
issue.
The present results are also very consistent qualitatively with
the theoretical predictions [26,27] suggesting that effective strain
is lesser in the SPD processes which involve strain reversal than in
(quasi)monotonic one. And therefore, rate of saturation in HABs
fraction and mechanical properties are retarded in them [27].
However, SPD processes that involve strain reversal are predicted
to produce UFG materials with higher ductility [26], and further
experimental work should be done to check this prediction.
The present investigation conrms that the strain reversal,
which takes place in most of the SPD methods, plays a signicant
role in structure evolution during SPD. Specically, it decreases the
rate of HABs formation at the stages of large strain accumulation.
This explains slower rate of the nanostructure formation of the SPD
methods that involve full strain reversal after each processing step,
e.g. ECAE by route C, MF, TE, CEC, etc. in comparison with HPT, ECAE
by routes A and B, and ARB. The present results suggest also that
the further, more detailed, studies on the effect of strain reversal on
the microstructure evolution in SPDand the mechanical properties
of the obtained materials should be done for deeper understanding
of the nanostructured metals. Numerical analysis of this effect is
also of great interest.
5. Conclusions
1. In this work, 99.99% purity aluminum was processed by high
pressure torsion to large strain values with two deformation
modes: monotonic and reversal. The effect of strain reversal on
intensity of grain renement under severe plastic deformation
was studied.
2. The strain reversal did not affect signicantly grain renement
and nal grain size, but signicantly retarded the formation of
high angle boundaries in comparison with monotonic straining.
The results explain slower rate of the nanostructure forma-
tion of the SPD processes that involve full strain reversal
after each consequent processing step in comparison with the
(quasi)monotonic techniques.
Acknowledgements
Authors of this work gratefully acknowledge nancial supports
by the Grant-in-Aid for scientic research from the ministry of
education on priority areas Giant straining process for advanced
materials containing ultra-high density lattice defects through the
Ministry of Education, Culture, Sports, Science and Technology of
Japan, and by Industrial Technology Research Grant Program05
through NEDO of Japan (project ID 05A27502d).
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