Materials Letters 290 (2021) 129462

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

The effect of initial strain in the severe plastic deformation of aluminum

on the subsequent work hardening regeneration through low strain
amplitude multi-directional forging
Cleber Granato de Faria a,b, Natanael Geraldo Silva Almeida a, Karla Balzuweit c,
Maria Teresa Paulino Aguilar d, Paulo Roberto Cetlin e,⇑
a
Graduate Program in Metallurgical, Materials and Mining Engineering, UFMG, Brazil
b
Centro Universitário Newton Paiva, Belo Horizonte, MG 30494-230, Brazil
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: Work hardening caused by Severe Plastic Deformation (SPD) strengthens ductile metals remarkably but
Received 5 December 2020 practically annihilates their further work hardening during monotonic post-SPD deformation. Low Strain
Received in revised form 25 January 2021 Amplitude Multi-Directional Forging (LSA-MDF) after one Equal Channel Angular Pressing (ECAP) pass of
Accepted 30 January 2021
aluminum causes limited softening and regenerates its work hardening capacity. The full development of
Available online 10 February 2021
an SPD condition in aluminum demands an initial deformation higher than that associated with one ECAP
pass. The present research analyzes the application of LSA-MDF to aluminum after 4 ECAP passes. A
Keywords:
regeneration of the work hardening capacity of the material was observed. In addition, LSA-MDF caused
Aluminum
Severe plastic deformation
an increased fraction of High Angle Grain Boundaries (HAGBs) in the material and a decrease in the pres-
Multi-directional forging ence of distorted grains displaying internal dislocation structures.
Microstructures Ó 2021 Elsevier B.V. All rights reserved.
Work hardening

1. Introduction
Ductile metals with Ultra Fine Grains (UFG) and high strength,
obtained through Severe Plastic Deformation (SPD), have been
receiving wide attention [1]. The observed remarkable strengthen-
ing is associated with the work hardening caused by the cold
deformation of the material. However, SPD causes undesirable
low or negative work hardening rates in subsequent monotonic
deformation [2]; relatively complex microstructural techniques
have been proposed in order to circumvent this difficulty [3], but
it has been recently shown that Low Strain Amplitude Multi-
Directional Forging (LSA-MDF) following one Equal Channel Angu-
lar Pressing (ECAP) regenerates the post-SPD work hardening of
99.77% aluminum [4] and is much simpler than the microstructural
routes. It was also found that LSA-MDF caused an accelerated
increase in the fraction of High Angle Grain Boundaries (HAGBs)
in the material, in comparison with successive SPD passes with
high strain amplitudes [5].
⇑ Corresponding author.
E-mail address: pcetlin@demec.ufmg.br (P.R. Cetlin).
Only one initial ECAP pass is insufficient to reach an UFG struc-
ture [1]. It is not known what would be the mechanical and
microstructural behavior of 99.77% aluminum submitted to a
higher number of ECAP passes followed by LSA-MDF. The objective
of the present paper is such a study, utilizing 4 initial ECAP passes.
A regeneration of the post-SPD work-hardening of the material
was obtained and the corresponding microstructural evolution
was analyzed.
2. Experimental
99.77% aluminum specimens underwent: 4 ECAP passes (strain
amplitude De-ECAP1.15, total strain 4.6) under route Bc, MDF
with confined dies (12 compressions, strain amplitude De-LSA =
0.075, total strain 0.9) and uniaxial monotonic compressions
(strain0.8). Details of these procedures have been described
elsewhere [4,6]. The material was evaluated in the following
conditions: (i) 4 ECAP passes (4ECAP) (ii) 4 ECAP passes and
compression (4ECAP + COMP) (iii) 4 ECAP passes and LSA-MDF
(4ECAP + LSA-MDF) and (iv) 4 ECAP passes, LSA-MDF and
compression (4ECAP + LSA-MDF + COMP). The microstructural
analyses involved Electron Backscattered Diffraction (EBSD) and

https://doi.org/10.1016/j.matlet.2021.129462
0167-577X/Ó 2021 Elsevier B.V. All rights reserved.
Cleber Granato de Faria, Natanael Geraldo Silva Almeida, K. Balzuweit et al.
Transmission Electron Microscopy (TEM) in the central region of
the specimen: cross-sections orthogonal to (i) the extrusion direc-
tion for 4ECAP, (ii) the first LSA-MDF compressed direction for the
4ECAP + LSA-MDF and (iii) the compression direction for the
4ECAP + COMP and 4ECAP + LSA-MDF + COMP, according to proce-
dures previously described [6]. EBSD data were processed with the
ATEX software. All experiments were performed in duplicate.
3. Results and discussion
Fig. 1 presents the stress-strain curves for the compression after
4ECAP, after 4ECAP + LSA-MDF and for the successive LSA-MDF
compressions in 4ECAP + LSA-MDF. In the compression after
4ECAP, the material yields at a stress ~160 MPa, softens slowly
down to ~155 MPa up to a strain ~0.4 (work softening rate of
5/0.4 = 12,5MPa) and then undergoes a mild work hardening
for the next straining of ~0.4, returning to the initial stress level
of ~160 MPa (work hardening rate of 5/0.4 = 12,5 MPa). The stres-
ses during each LSA-MDF compression rise abruptly after the spec-
imens touches the lateral walls of the die and the stress state is no
more uniaxial [6]. LSA-MDF causes a gradual softening of the mate-
rial down to a flow stress ~128 MPa (a ~20% reduction in relation to
the yield stress of the material after 4ECAP, at a work softening rate
of 32/0.9 = 35.5 MPa, far stronger than under monotonic com-
pression). Compression after 4ECAP + LSA-MDF exhibits a positive
work hardening, from an initial flow stress of ~128 MPa up to a
flow stress of ~150 MPa after a straining of ~0.8; (work hardening
rate of 22/0.8 = 27,5MPa, much higher than in the previously
described softening/hardening situations). LSA-MDF thus also
regenerates the work hardening capacity of material previously
submitted to 4ECAP passes, similarly to the situation after 1ECAP
pass [4]. It is additionally remarkable that the work hardening rate
for compression after 4ECAP + LSA-MDF is constant over the full
~0.8 strain span, a behavior far unusual for metals, where work
hardening is typically parabolic.
Fig. 2 displays the Orientation Imaging Maps (OIM), where
black lines correspond to boundaries with disorientations >15°
(High Angle Grain Boundaries – HAGBs), and Grain Disorientation
Maps for the various present material conditions. Fig. 2a (4ECAP)
shows regions with color hues, indicating the presence of disloca-
tion cells/sub-grains with boundary disorientations 15° (Low
Angle Grain Boundaries - LAGBs), as confirmed in Fig. 2b. Fig. 2c
and d (4ECAP + COMP) display a more uniform microstructure
Fig. 1. Stress strain curves for the compression of the material after 4ECAP, after 4ECAP + LSA-MDF and during LSA-MDF.
2
Materials Letters 290 (2021) 129462
and where regions surrounded by HAGBs are larger than after
4ECAP. Material after 4ECAP + LSA-MDF (Fig. 2e and f) exhibits a
microstructure with sizes similar to those after 4ECAP but with a
higher fraction of HAGBs. LSA-MDF thus eliminated most of the
LAGBs in the material after 4ECAP, which evolved into HAGBs.
Finally, material submitted to 4ECAP + LSA-MDF + COMP (Fig. 2g
and h) shows a decrease in the HAGBs fraction and an increase
in the size of the regions surrounded by these boundaries. In addi-
tion, the observed microstructures are somewhat more heteroge-
neous than under 4ECAP + LSA-MDF.
The fraction of HAGBs after 4ECAP was ~0.541, similarly to that
reported for pure Al [7], which increased by 0.144 (up to ~0.685)
after the application of LSA-MDF. Such increase is approximately
the same observed for the application of LSA-MDF after 1ECAP
(0.117, from ~0.134 to ~0.251) [5]). It has been reported [8] that
the HAGB fraction of pure aluminum increases very slowly for fur-
ther deformation after 4ECAP passes [8] and a total deformation of
~12 was necessary to reach a HAGB fraction similar to that pre-
sently reported for 4ECAP + LSA-MDF (total strain 4.6 + 0.9 = 5.5)
. Previous results [5], indicating the capacity of LSA-MDF to accel-
erate the formation of HAGBs, in comparison with the application
of high strain amplitude ECAP passes, are thus confirmed.
Material after 4ECAP + COMP displayed a HAGBs fraction of
~0.495, a decrease of 0.046 from the ~0.541 fraction after 4ECAP
passes. The application of compression after 4ECAP + LSA-MDF
lowers the HAGBs fraction from ~0.685 to ~0.544 (a decrease of
0.141); compression after 1ECAP + LSA-MDF caused a decrease in
the HAGBs fraction of 0.128 (from 0.251 down to 0.123) [5]. The
decrease in the HAGBs fraction caused by compression thus
depends on the nature of the initial microstructure of the material.
Structures generated by 1ECAP + LSA-MDF or by 4ECAP + LSA-MDF
led to a higher reduction in the HAGBs fraction caused by compres-
sion than structures generated by ECAP alone, and this is probably
the cause of the regeneration in work hardening capacity of the
material associated with the application of LSA-MDF.
Fig. 3 displays TEM images for the same conditions as in Fig. 2.
Grains after 4ECAP (Fig. 3a and b), exhibit heterogeneous sizes and
occasionally display internal dislocations substructures. The com-
pression of this material (Fig. 3c and d) causes distorted grains
and an increase in the presence of grains with internal dislocation
structures, as well as an increase in grain sizes, as already observed
in EBSD results. On the other hand, LSA-MDF after 4ECAP (Fig. 3e
and f) leads to quite homogeneous grain sizes and an almost com-
plete absence of internal dislocation structures inside these grains.
Cleber Granato de Faria, Natanael Geraldo Silva Almeida, K. Balzuweit et al. Materials Letters 290 (2021) 129462

Fig. 2. Orientation Imaging Maps (OIM), where black lines correspond to boundaries with grain disorientations >15°, and Grain Disorientation Maps for the various present
material conditions.

3
Cleber Granato de Faria, Natanael Geraldo Silva Almeida, K. Balzuweit et al.
Fig. 3. TEM images after processing by: (a, b) 4ECAP; (c, d) 4ECAP + COMP; (e, f) 4ECAP + LSA-MDF; (g, h) 4ECAP + LSA-MDF + COMP.
The compression of this material (Fig. 3g and h) has an effect sim-
ilar to that observed for 4ECAP + COMP: distorted grains frequently
exhibiting internal dislocation structures.
Both compressions, either after 4ECAP or 4ECAP + LSA-MDF,
cause grain distortions and a re-structuring of their boundaries,
connected to the migration of boundary dislocations to the interior
of the grains. LSA-MDF, on the other hand, consistently promotes
4
Materials Letters 290 (2021) 129462
the decrease of dislocation structures inside the grains and an
increase in undistorted boundaries, connected to the observed
increase in the HAGBs fraction. These TEM results are in line with
those from EBSD.
The softening promoted by LSA-MDF processing after 4ECAP
reached ~32 MPa (a softening of ~20%). On the other hand, mono-
tonic compression after 4ECAP caused an initial softening far lower
Cleber Granato de Faria, Natanael Geraldo Silva Almeida, K. Balzuweit et al.
than that caused by LSA-MDF, followed by a very slow work hard-
ening, totaling practically no softening. The microstructural obser-
vations indicate that whereas LSA-MDF after 4ECAP caused an
increase in the HAGBs fraction and a decrease in the presence of
distorted grains displaying internal dislocation structures, com-
pression after 4ECAP caused an increase in the (i) size of regions
surrounded by HAGBs, (ii) presence of grain boundary distortions
and (iii) the presence of grains displaying internal dislocation
structures, as well as a small decrease in the HAGB fraction. The
initial modest softening during compression after 4ECAP seems
to be associated with an initial structural re-organization leading
to growth of regions surrounded by HAGBs, followed by a stabiliza-
tion of this structure, On the other hand, softening caused by LSA-
MDF is connected to an increase in the HAGBs fraction coupled to a
decrease in the presence of grains displaying distorted boundaries
and internal dislocation boundaries.
4. Conclusions
The application of LSA-MDF to SPD processed material
deformed by ECAP causes softening and work hardening capacity
regeneration for both initial 1 and 4ECAP passes. These phenomena
are associated with a decrease in the presence of grain boundary
distortions, of grains displaying dislocation structures in their
internal regions and with an increase in the fraction of HAGBs.
CRediT authorship contribution statement
Cleber Granato de Faria: Investigation, Supervision, Formal
analysis, Writing - original draft, Writing - review & editing, Vali-
dation. Natanael Geraldo Silva Almeida: Investigation, Formal
analysis, Writing - original draft, Validation. Karla Balzuweit: Data
curation, Writing - review & editing, Methodology. Maria Teresa
Paulino Aguilar: Supervision, Data curation, Writing - review &
editing, Formal analysis, Methodology. Paulo Roberto Cetlin:
Supervision, Conceptualization, Data curation, Writing - review &
editing, F, unding acquisition, Project administration.
Materials Letters 290 (2021) 129462
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
Material was supplied by Novelis do Brasil. Coordenação de
Aperfeiçoamento de Pessoal de Nível Superior - Brasil (CAPES) -
Finance Code 001 and CNPq (National Council for Research and
Technological Development) Grant 300874/2018-9 financed this
research. Electron microscopy experiments were performed in
the Center of Microscopy at the Universidade Federal de Minas
Gerais, Belo Horizonte, MG, Brazil (http://www.microscopia.ufmg.
br).
References
[1] R.Z. Valiev, Y. Estrin, Z. Horita, T.G. Langdon, M.J. Zehetbauer, Y.T. Zhu,
Fundamentals of superior properties in bulk nanoSPD materials, Mater. Res.
Lett. 4 (1) (2016) 1–21, https://doi.org/10.1080/21663831.2015.1060543.
[2] Y. Cao, S. Ni, X. Liao, M. Song, Y. Zhu, Structural evolutions of metallic materials
processed by severe plastic deformation, Mater. Sci. Eng. R Rep. 133 (2018) 1–
59, https://doi.org/10.1016/j.mser.2018.06.001.
[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, https://doi.org/10.1016/j.msea.2012.09.020.
[4] C.G. de 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,
https://doi.org/10.1016/j.matlet.2016.03.112.
[5] C.G. de Faria, B.F. de Castro, K. Balzuweit, M.T.P. Aguilar, P.R. Cetlin,
Microstructural evolution in the low strain amplitude multi-axial
compression (LSA-MAC) after equal channel equal pressing (ECAP) of
aluminum, Mater. Lett. 227 (2018) 149–153, https://doi.org/10.1016/
j.matlet.2018.05.054.
[6] N.G.S. Almeida, P.H.R. Pereira, C.G.d. Faria, M.T.P. Aguilar, P.R. Cetlin, Mechanical
behavior and microstructures of aluminum processed by low strain amplitude
multi-directional confined forging, J. Mater. Res. Technol. 9 (3) (2020) 3190–
3197, https://doi.org/10.1016/j.jmrt.2020.01.065.
[7] T.G. Langdon, Twenty-five years of ultrafine-grained materials: Achieving
exceptional properties through grain refinement, Acta Mater. 61 (2013) 7035–
7059.
[8] M. Kawasaki, Z. Horita, T.G. Langdon, Microstructural evolution in high purity
aluminum processed by ECAP, Mater. Sci. Eng. A 524 (1-2) (2009) 143–150,
https://doi.org/10.1016/j.msea.2009.06.032.