Materials Letters 227 (2018) 149–153

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Materials Letters
journal homepage: www.elsevier.com/locate/mlblue

Microstructural evolution in the low strain amplitude multi-axial

compression (LSA-MAC) after equal channel equal pressing (ECAP) of
aluminum
Cleber Granato de Faria a, Natanael Geraldo e Silva Almeida a, Franco de Castro Bubani b, Karla Balzuweit c,
Maria Teresa Paulino Aguilar d, Paulo Roberto Cetlin e,⇑
a
Graduate Program in Metallurgical, Materials and Mining Engineering, UFMG, Brazil
b
CAB(CONICET) and Universidad Nacional de Cuyo, Argentina
c
Dept. of Physics, UFMG, Brazil
d
Dept of Construction and Materials, UFMG, Brazil
e
Dept of Mechanical Engineering, UFMG, Brazil

a r t i c l e i n f o a b s t r a c t

Article history: Low strain amplitude multi-axial compression (LSA-MAC) increases the work hardening capacity and
Received 22 April 2018 uniform ductility of Aluminum after Severe Plastic Deformation (SPD) through Equal Channel Angular
Received in revised form 9 May 2018 Pressing (ECAP). The mechanisms associated with this processing after ECAP are analyzed. LSA-MAC after
Accepted 11 May 2018
1 ECAP pass in Aluminum softens the material and is connected to the stabilization of the dislocation
Available online 17 May 2018
structures induced by ECAP into a configuration displaying an increased fraction of High Angle Grain
Boundaries (HAGB). This occurs for a lower total imposed strain than that through a sequence of high
Keywords:
strain ECAP passes or high strain amplitude multi-axial compression (HAS-MAC).
Metals and alloys
Equal Channel Angular Pressing (ECAP)
Ó 2018 Elsevier B.V. All rights reserved.
Low strain amplitude multi-axial
compression (LSA-MAC)
Severe Plastic Deformation (SPD)
Work hardening
Microstructures

1. Introduction
The production of ultrafine-grained (UFG), high strength metals,
through Severe Plastic Deformation (SPD) usually employs Equal
Channel Angular Pressing (ECAP), High Pressure Torsion (HPT) or
High Strain Amplitude (De) Multi-Axial Compression (HSA-MAC,
De  0.5–0.8), [1] also widely known as Multi-Directional Forging
(MDF) [2]. UFG materials exhibit low or negative work hardening
rate and a low tensile uniform elongation after processing.
Microstructural changes in the material before SPD have been
developed for increasing their post-SPD low work hardening
capacity [3]. A recent study by the present authors [4] showed
that Low Strain Amplitude Multi-Axial Compression (LSA-MAC,
De = 0.075) after ECAP led to an increase in the work hardening
capacity of aluminum; this is simpler than pre-SPD microstructural
manipulations and can be used for all materials. The present objec-
tive is to analyze the microstructural aspects connected to this new
procedure. The results indicate that the effects of LSA-MAC after
⇑ Corresponding author.
E-mail address: pcetlin@gmail.com (P.R. Cetlin).
ECAP are associated with the stabilization of the dislocation struc-
tures after a much lower total strain than that observed in the
usual SPD techniques.
2. Experimental
As-cast 1070 Aluminum specimens underwent: 1 ECAP pass,
annealing, another ECAP pass, LSA-MAC (12 compressions, De =
0.075) and simple compression. Detailed experimental procedures
have been described elsewhere [4]. The material was evaluated in
the following conditions: (i) as-cast, 1 ECAP pass and annealed
(An) (ii) annealed and 1 ECAP pass (An+ECAP) (iii) annealed, 1
ECAP pass and LSA-MAC (An+ECAP+LSA-MAC) (iv) annealed, 1
ECAP pass, LSA-MAC and compression (An+ECAP+LSA-MAC
+COMP). The analyses involved microhardness testing, Electron
Backscattered Diffraction (EBSD) and Transmission Electron Micro-
scopy (TEM) in the specimen cross-section orthogonal to (i) the
extrusion direction for An and An+ECAP, (ii) the first compressed
direction for the An+ECAP+LSA-MAC and (iii) the compression
direction for the An+ECAP+LSA-MAC+COMP. Vickers microhard-
ness employed a Mitutoyo MVK-H1 with a 500 g load for 15 s;

https://doi.org/10.1016/j.matlet.2018.05.054
0167-577X/Ó 2018 Elsevier B.V. All rights reserved.
150 C.G. de Faria et al. / Materials Letters 227 (2018) 149–153
surface preparation involved initial 600 mesh paper, electrolytic
polishing (700 ml C2H5OH, 120 ml distilled H2O, 100 ml C4H9OC2-
H4OH, 68 ml 70% HClO4 at 35 V for 45 s and a stainless steel cath-
ode). 20 measurements were taken at evenly distributed points in
the specimen section. EBSD and TEM were performed in the central
part of the above mentioned cross-sections. At least 3 different
areas were analyzed for each processing condition; since no
remarkable differences were observed for these different areas,
one of them was chosen as a typical one for the present paper.
TEM employed a Tecnai G2-20 SuperTwin FEI-200 kV (UFMG) or
a Philips CM200 Ultratwin–200 kV (Bariloche); specimens were
ground to a thickness of 100 mm, punched into 3 mm diameter
discs and perforated with a double jet TENUPOL 5 using a 30%
nitric acid–methanol solution at 243 K. EBSD specimens were pre-
pared similarly to those for microhardness. A Quanta FEG 3D FEI
SEM with a Bruker QUANTAX EBSD analysis system was utilized.
Data were processed with the Bruker Esprit 2 software. Detection
of neighboring grains was set at a disorientation angle of 2°. For
the large grained An specimen the area was 30820 mm2 and step
size 270 nm; for the other conditions, the area was 4802 mm2 and
step size 62 nm. 98.5% and 90% of the points were indexed for
the An specimen and for the other specimens, respectively. Noise
elimination completed the absent indexing for some points,
through an averaging from neighboring points.
3. Results and discussion
The average microhardness for the various conditions were: An:
21.2 ± 1.7HV, An+ECAP: 45.3 ± 2.9HV, An+ECAP+LSA-MAC: 36.5 ±
1.8HV, An+ECAP+LSA-MAC+COMP: 40.9 ± 2.0HV. LSA-MAC after
the ECAP softens the material, whereas the final compression step
hardens it again, in line with a previous report [4].
Fig. 1 displays the Orientation Imaging Microscopy (OIM)
results for the conditions: (a) An, (b) An+ECAP, (c) An+ECAP
Fig. 1. OIM images for specimens in the conditions: (a) An, (b) An+ECAP, (c) An+ECAP+LSA-MAC and (d) An+ECAP+LSA-MAC+COMP.
+LSA-MAC and (d) An+ECAP+LSA-MAC+COMP. The An grains
(Fig. 1a) are approximately equiaxed and single colored. The An
+ECAP condition (Fig. 1b) exhibits large and small elongated
grains; the former correspond to the original An grains and display
color hues, connected to regions with small disorientations, indi-
cating the presence of dislocation cells/subgrains. The additional
strain imposed by LSA-MAC after ECAP increases the fraction of
areas with small elongated grains (Fig. 1c), often fragmented along
their lengths. LSA-MAC caused a fast evolution of initial grains
towards equiaxed UFGs due to the variation in the shearing planes
associated with the changes in the compression direction [5], sim-
ilarly to the Bc route in ECAP [6]. The microstructure for the An
+ECAP+LSA-MAC+COMP condition (Fig. 1d) displays color hues,
similarly to the situation after ECAP, indicating the presence of
cell/subgrains.
Fig. 2 displays the grain boundary characteristics and disorien-
tation distributions for the conditions, respectively: (a and b) An, (c
and d) An+ECAP, (e and f) An+ECAP+LSA-MAC and (g and h) An
+ECAP+LSA-MAC+COMP. Comparing Fig. 2a and b with Fig. 2c
and d indicates that ECAP refined the grains, displaying a predom-
inance of grain disorientations in the range of 2° to 5° (0.637). ECAP
also leads to a fraction of 0.866 LAGB (disorientation angles < 15°),
similarly to reports in the literature [7,8]. Fig. 2e and f show that
LSA-MAC decreased the fraction of grain boundaries with
disorientations in the range of 2–5° (0.639 after ECAP, 0.496 after
LSA-MAC), coupled to an increase in the fraction of HAGBs (grain
disorientation >15°) from 0.134 after ECAP to 0.251 after LSA-
MAC. Compression after ECAP+LSA-MAC is connected to a grain
disorientation distribution similar to that after ECAP (Fig. 2g
and h, HAGB fraction of 0.123), reverting the tendency of increased
HAGB fraction caused by LSA-MAC.
Fig. 3 displays TEM images for the conditions: (a and b) An
+ECAP, (c and d) An+ECAP+LSA-MAC and (e and f) An+ECAP
+LSA-MAC+COMP. An+ECAP material displays elongated and
equiaxed grains with internal dislocations (Fig. 3a and b), similarly
 C.G. de Faria et al. / Materials Letters 227 (2018) 149–153 151

Fig. 2. Grain boundary characteristics and grain disorientation distributions for specimens: (a and b) An, (c and d) An+ECAP, (e and f) An+ECAP+LSA-MAC and (g and h) An
+ECAP+LSA-MAC+COMP.

to the literature [6]. The grains for the An+ECAP+LSA-MAC
condition (Fig. 3e and f) are more equiaxed and somewhat smaller
than those after An+ECAP; displaying intragranular dislocation
structures (see the lower right corner, Fig. 3c). Compression after
LSA-MAC (An+ECAP+LSA-MAC+COMP, Fig. 3e and f) lead to grain
sizes somewhat larger than for An+ECAP+LSA-MAC (Fig. 3c and
d), but without any remarkable differences.
SPD initially forms dislocation tangles and cell walls; that thin
and evolve into more stable and lower energy dislocation config-
urations such as HAGBs [9] as strain rises. This is observed in Alu-
minum after 4 ECAP passes [10] and after 6 high strain amplitude
Multi-axial compression (HSA-MAC) cycles with strain amplitude
De = 0.80 [11]. The strength of Copper decreases after more than
4 ECAP passes stabilizes up to 16 ECAP passes [12]. This is also
152 C.G. de Faria et al. / Materials Letters 227 (2018) 149–153

Fig. 3. TEM images for the following conditions: (a and b) An+ECAP, (c and d) An+ECAP+LSA-MAC and (e and f) An+ECAP+LSA-MAC+COMP.

reported for the compression in the transversal direction of Cop- 4. Conclusions

per after ECAP and Aluminum after 2 ECAP passes [10]. Softening
also occurs in Copper [13] and Aluminum [11] in plane strain SPD through ECAP and high strain amplitude multi-axial com-
HSA-MAC after strains of ~4–5, both for a strain amplitude De pression (HSA-MAC, De  0.5–0.8) stabilizes the dislocation struc-
= 0.8. Data for Copper show that, as the number of ECAP passes tures after a large total strain and number of deformation steps.
is raised up to 16, grain size decreases up to 1–2 ECAP passes, fol- Low strain amplitude multi-axial compression (LSA-MAC, De =
lowed by grain size stabilization; HAGB/unit area increases up to 0.075) after ECAP accelerates, in terms of a lowered total imposed
about 12 passes and slowly decreases up to the 16th pass. Dislo- strain, the stabilization of the dislocation structures into lower
cation density rises up to the 4th pass and slowly decreases and energy arrangements, leading to softening and increased work
stabilizes up to the 16th pass [14]. hardening capacity of the material for further monotonic straining.
The present results show that a straining of 1.15 by ECAP fol-
lowed by LSA-MAC with a total strain of 0.9 (12 steps, De = 0.0
Acknowledgments
75), totaling a strain of 2.05, led to an HAGB fraction of 0.251,
similarly to that for an ECAP strain of 3 in Al 99,99% [7] and
The authors are grateful for the financial support of the Brazil-
4 in Al 1%Mg [8], and to a strain 4.6 in the HSA-MAC of Alu-
ian Education Ministry, through the CAPES/PROEX and PROF pro-
minum [11] and to a decrease in the material hardness. ECAP
grams of the Graduate Program in Metallurgical and Materials
+LSA-MAC causes effects similar to those described above for
Engineering at UFMG and of MCTI/CNPq and FAPEMIG.
Copper [13,14] and Aluminum [11], for a much lower total strain
than those reported in the literature. The monotonic compression
after ECAP+LSA-MAC interrupted the increase in the HAGB frac- References
tion caused by LSA-MAC after ECAP and reversed the evolution
[1] R.Z. Valiev, R.K. Islamgaliev, I.V. Alexandrov, Bulk nanostructured materials
of this fraction. from severe plastic deformation, Prog. Mater. Sci. 45 (2000) 103–189.
 C.G. de Faria et al. / Materials Letters 227 (2018) 149–153
[2] Y. Estrin, A. Vinogradov, Extreme grain refinement by severe plastic
deformation: a wealth of challenging science, Acta Mater. 61 (2013) 782–817.
[3] I. Sabirov, M.Y. Murashkin, R.Z. Valiev, Nanostructured aluminium alloys
produced by severe plastic deformation: New horizons in development, Mater.
Sci. Eng. A 560 (2013) 1–24.
[4] C.G. Faria, N.G.S. Almeida, M.T.P. Aguilar, P.R. Cetlin, Increasing the
work hardening capacity of equal channel angular pressed (ECAPed)
aluminum through multi-axial compression (MAC), Mater. Lett. 174 (2016)
153–156.
[5] T. Sakai, H. Miura, X. Yang, Ultrafine grain formation in face centered cubic
metals during severe plastic deformation, Mater. Sci. Eng. A 499 (2009) 2–6.
[6] T.G. Langdon, The principles of grain refinement in equal-channel angular
pressing, Mater. Sci. Eng. A 46 (2007) 3–11.
[7] M. Kawasaki, Z. Horita, T.G. Langdon, Microstructural evolution in high purity
aluminum processed by ECAP, Mater. Sci. Eng. 524 (2009) 143–150.
[8] C. Xu, Z. Horita, T.G. Langdon, Microstructural evolution in an aluminum solid
solution alloy processed by ECAP, Mater. Sci. Eng. A 528 (2011) 6059–6065.
153
[9] R.Z. Valiev, Y.V. Ivanisenko, E.F. Rauch, B. Baudelet, Structure and deformaton
behaviour of Armco iron subjected to severe plastic deformation, Acta Mater.
44 (1996) 4705–4712.
[10] I.J. Beyerlein, D.J. Alexander, C.N. Tomé, Plastic anisotropy in aluminum and
copper pre-strained by equal channel angular extrusion, J. Mater. Sci. 42
(2007) 1733–1750.
[11] R. Kapoor, A. Sarkar, R. Yogi, S.K. Shekhawat, I. Samajdar, J.K. Chakravartty,
Softening of Al during multi-axial forging in a channel die, Mater. Sci. Eng. A
560 (2013) 404–412.
[12] F. Dalla Torre, R. Lapovok, J. Sandlin, P.F. Thomson, C.H.J. Davies, E.V. Pereloma,
Microstructures and properties of copper processed by equal channel angular
extrusion for 1–16 passes, Acta Mater. 52 (2004) 4819–4832.
[13] A. Kundu, R. Kapoor, R. Tewari, J.K. Chakravartty, Severe plastic deformation of
copper using multiple compression in a channel die, Scr. Mater. 58 (2008)
235–238.
[14] H.J. Maier, P. Gabor, N. Gupta, I. Karaman, M. Haouaoui, Cyclic stress-strain
response of ultrafine grained copper, Int. J. Fatigue 28 (2006) 243–250.