Materials Science and Engineering A 398 (2005) 66–76

The evolution of homogeneity and grain refinement during equal-channel

angular pressing: A model for grain refinement in ECAP
Cheng Xu a , Minoru Furukawa b , Zenji Horita c , Terence G. Langdon a,∗
aDepartments of Aerospace & Mechanical Engineering and Materials Science, University of Southern California,
Los Angeles, CA 90089-1453, USA
b Department of Technology, Fukuoka University of Education, Munakata, Fukuoka 811-4192, Japan
c Department of Materials Science and Engineering, Faculty of Engineering, Kyushu University, Fukuoka 812-8581, Japan

Received 2 November 2004; received in revised form 17 February 2005; accepted 16 March 2005

Abstract

Samples of pure aluminum and an Al-6061 alloy were subjected to equal-channel angular pressing (ECAP) for up to eight passes at room
temperature. The Vickers microhardness was recorded on the polished cross-sections of each as-pressed billet and the results are plotted in
the form of color-coded maps to provide a pictorial depiction of the hardness distributions throughout the cross-sections. The results show
the hardness increases by a factor of ∼2 in the first pass through the die but thereafter there is only a minor increase. The microhardness
distribution is homogeneous in the unpressed condition but becomes inhomogeneous after a single pass and then reasonably homogeneous in
subsequent passes. The results reveal some differences between the behavior of pure Al and the Al-6061 alloy. These results and microscopic
observations are used to develop a model for the process of grain refinement during ECAP.
© 2005 Elsevier B.V. All rights reserved.

Keywords: Equal-channel angular pressing; Grain refinement; Hardness; Homogeneity; Severe plastic deformation

1. Introduction ing (ECAP) in which a metallic rod or bar is pressed through

The processing of metals through the application of severe
plastic deformation (SPD) has become attractive in recent
years, because it provides the capability of achieving remark-
able grain refinement in polycrystalline materials, typically
to the submicrometer or even the nanometer level [1]. There
are two primary advantages of using SPD processing. First, it
has a potential for producing large bulk samples without the
introduction of any porosity or the contaminants that are often
inherent in alternative techniques such as inert gas conden-
sation or ball milling. Second, conventional SPD processing
can be applied relatively easily to a wide range of metallic
alloys without making any significant changes in the process-
ing procedure.
The most attractive, and potentially the most useful,
SPD technique appears to be equal-channel angular press-
∗ Corresponding author. Tel.: +1 213 740 0491; fax: +1 213 740 8071.
E-mail address: langdon@usc.edu (T.G. Langdon).
a die constrained within a channel which is bent through an
abrupt angle that is often equal to, or very close to, 90◦ [2–4].
Processing by ECAP leads to significant strengthening of
the material at ambient temperatures [5,6] and, provided the
ultrafine grains have a reasonable thermal stability, to the oc-
currence of superplastic ductilities at very rapid strain rates
at elevated temperatures [7,8].
Despite the apparent success in producing both high
strength and high strain rate superplasticity in materials
processed by ECAP, it is important to recognize that the
tensile specimens used to establish these mechanical prop-
erties are generally cut from the as-pressed billets with their
gauge lengths lying parallel to the longitudinal or pressing
axes. This means, in effect, that the measured mechanical
properties represent the characteristics associated with the
as-pressed microstructure existing within the central core
regions of the as-pressed billets and the mechanical testing
provides no information on the general degree of microstruc-
tural homogeneity occurring in the cross-sections of the

0921-5093/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2005.03.083
 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76
billets perpendicular to the pressing axis. An earlier study
demonstrated the feasibility of effectively scaling the ECAP
process to include billets having diameters from 6 to 40 mm
[9] and in these experiments some tensile specimens, having
gauge lengths of 5 mm, were cut from the 40 mm billet with
their gauge lengths oriented in two mutually orthogonal
directions perpendicular to the pressing direction. Although
the subsequent curves of stress versus strain were essentially
identical for all of these tensile specimens and for other
specimens cut parallel to the pressing direction, thereby
suggesting a reasonably homogeneous microstructure, the
results are insufficient to provide detailed information on
either the degree of homogeneity within the cross-sections or
the changes in any inhomogeneities with increasing numbers
of passes through the die. This information is necessary
because the microstructure may change in the vicinity of
the die walls if, for example, frictional effects become
important.
The present investigation was initiated with three objec-
tives. First, to use hardness measurements to evaluate the
homogeneity of the microstructures on sections cut through
the as-pressed billets perpendicular to the pressing direction.
Second, to evaluate the significance of any evolution in the
microstructural homogeneity as a function of the number of
passes in ECAP and hence of the imposed strain. Third, to
make use of these observations, together with earlier reports
of microstructural development in ECAP, in order to construct
a model to account for the evolution of an ultrafine-grained
structure when processing by ECAP.
The experiments were conducted using two different ma-
terials: high-purity aluminum and an Al-6061 alloy. These
materials were selected because there are several earlier stud-
ies documenting the basic characteristics of high-purity alu-
minum [10–15] and the Al-6061 alloy [16] when processing
using ECAP. As will be demonstrated, there are microstruc-
tural inhomogeneities in both of these materials after ECAP
through a single pass but the microstructures evolve with ad-
ditional passes and, except only for very small regions in the
vicinity of the bottom surfaces of the billets, they become
essentially homogeneous in both materials.
2. Experimental materials and procedures
The experiments were conducted using pure aluminum of
99.99% purity and a commercial Al-6061 alloy containing,
in wt.%, 1.01% Mg, 0.59% Si, 0.37% Fe, 0.29% Cu, 0.23%
Cr and 0.20% Zn.
The aluminum was prepared by cold-rolling from an in-
got into a plate with a thickness of 25 mm, cutting into a
block with cross-sectional dimensions of 25 mm × 25 mm
and swaging into cylindrical rods having diameters of 10 mm.
For processing by ECAP, individual billets were cut from
these rods with lengths of ∼70 mm. These billets were an-
nealed at 773 K for 1 h prior to ECAP to give an initial un-
pressed grain size of ∼1 mm.
67
The Al-6061 alloy was received in the form of a plate,
10 mm in thickness, after a T651 heat treatment involving
a solution treatment at 823 K, tensile straining to ∼2% at
room temperature and aging at 433 K for 18 h. Samples with
diameters of 10 mm and lengths of 70 mm were cut from
the plate and annealed at 693 K for 4 h with a heating and
cooling rate of 10 K h−1 . The initial grain size of the alloy in
the unpressed condition was ∼50 ␮m.
The ECAP processing for both materials was performed
at room temperature (298 K) using a hydraulic press of
150 tonnes capacity operating at a ram speed of ∼7 mm s−1 .
The pressings were conducted using a solid die having an
L-shaped channel bent through an angle of Φ = 90◦ near the
center of the die and with an additional angle of Ψ = 20◦ rep-
resenting the outer arc of curvature where the two parts of
the channel intersect. These values of Φ and Ψ lead to an im-
posed strain of ∼1 on each passage of the sample through the
die [17]. An earlier investigation, also conducted using pure
Al, showed that the use of a solid die with an arc of curvature
of Ψ = 20◦ has no significant influence on measurements of
homogeneity in the as-pressed samples by comparison with a
conventional split die where the channel is bent through 90◦
and there is no arc of curvature so that Ψ = 0◦ [18]. Samples
were processed by ECAP through selected numbers of passes
using route BC in which the samples are rotated by 90◦ in the
same sense between each pass [19]. This processing route
was selected because earlier experiments on high-purity Al
showed it leads most expeditiously to an array of equiaxed
grains separated by boundaries having high angles of misori-
entation [12].
Following ECAP, the billets were sectioned perpendic-
ular to their longitudinal axes and then mounted and care-
fully polished to a mirror-like finish. Microhardness mea-
surements were taken using an FM-1e microhardness tester
equipped with a Vickers indenter. A series of individual mea-
surements was recorded on each polished section whereby
the Vickers indenter was moved over the surface and mea-
surements of the Vickers microhardness, Hv, were recorded
in a regular grid pattern with spacings between each sepa-
rate measurement of ∼0.5 mm. This procedure gave a total
of ∼220 individual values of Hv on each polished section.
These individual values of Hv were then plotted in the form
of color-coded contour maps depicting the variation of the
local microhardness over the cross-sectional plane for each
sample.
The internal microstructures of pure Al were examined
using an Hitachi H-8100 transmission electron microscope
(TEM) operating at 200 kV. Specimens were prepared for
TEM in the form of disks, 3 mm in diameter, oriented in the
plane of sectioning perpendicular to the longitudinal axes of
the billets. These disks were ground mechanically to thick-
nesses of ∼150 ␮m and then thinned to perforation using
a twin-jet electropolishing facility with a solution of 10%
HClO4 , 20% C3 H8 O3 and 70% C2 H5 OH with the solution
maintained at a temperature of 278 K. Observations were
recorded by TEM both in the central regions of the billets
68 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76
Fig. 1. The average Vickers microhardness, Hv, vs. the number of passes in
ECAP for pure aluminum and an Al-6061 alloy processed at room temper-
ature using route BC .
and in the vicinity of the lower surface. The grain sizes were
measured in the TEM and selected area electron diffraction
(SAED) patterns were recorded using an aperture size of
12.3 ␮m.
3. Experimental results
3.1. The variation of the average microhardness with
strain
The value of the Vickers microhardness, Hv, was deter-
mined for each billet by calculating the average of all mi-
crohardness measurements on each plane of sectioning. The
results are plotted in Fig. 1 against the total number of passes
in ECAP corresponding to imposed strains up to a maxi-
mum of ∼8. It is important to note that the error bars associ-
ated with these points are extremely small because each point
represents the average of ∼220 individual readings. Table 1
records the error bars at the 95% confidence limit and it can
be seen the errors in the values of Hv are consistently <1 and
in practice they are smaller than the size of the individual
datum points plotted in Fig. 1.
It is apparent from Fig. 1 that the microhardness of
both materials increases dramatically after a single pass of
ECAP by a factor of approximately 2×. Thereafter, there
is a small increase in each additional pass for the Al-6061
alloy up to a maximum value of Hv ≈ 99 after six passes
whereas for pure Al there is a very small increase in the
Table 1
Average values of the microhardness and errors at the 95% confidence level for pure Al and the Al-6061 alloy
Material Pass number
0 1 2 3
Pure Al 18.6 ± 0.1 40.4 ± 0.6 44.1 ± 0.5
Al-6061 44.7 ± 0.2 77.9 ± 0.6 85.4 ± 0.7
second pass to a maximum value of Hv ≈ 44 and then a
slight decrease to a value of Hv ≈ 42 after a total of eight
passes.
3.2. Distribution of microhardness through
cross-sections of the billets
3.2.1. Pure aluminum
All of the microhardness measurements were plotted in
the form of contour maps depicting, within incremental steps,
the locations of individual microhardness values on the cross-
sectional planes. In plotting these maps, the positions of the
microhardness measurements were taken from the rectilin-
ear coordinate system used in the experiments with the Y
and the Z axes defined as the directions tangential to the
top point and the side point of the circular cross-section of
the billet at the point of exit from the die, respectively: fol-
lowing the coordinate system introduced earlier for ECAP
[11], this corresponds to directions perpendicular to the flow
(Y) and longitudinal (Z) planes, respectively. The distribu-
tions of the microhardness values are represented pictori-
ally through a series of colors defined within these incre-
mental values of Hv, thereby giving a direct and visual
presentation of the sample homogeneity before and after
ECAP.
Fig. 2 shows the color-coded hardness maps for pure Al
where the number of passes is indicated above each display
and the meanings of the colors are given at the lower right. The
map at upper left in Fig. 2 shows the as-received condition
immediately prior to ECAP and it is apparent that the values
of Hv, having an average value of Hv ≈ 19, are essentially
independent of the location on the section thereby confirming
the presence of a reasonably homogeneous microstructure
throughout the billet.
The contour maps obtained after processing by ECAP
are shown in the remaining displays. Two conclusions may
be drawn from the display at upper right for a single pass
in ECAP. First, the microhardness after one pass is sig-
nificantly higher than in the unpressed condition and this
increase has occurred over the entire section of the bil-
let so that there is no region where the microhardness re-
mains at, or even close to, Hv ≈ 19. Second, the distribu-
tion of the microhardness measurements is less homoge-
neous than in the unpressed condition and there is a broad
region in the vicinity of the lower surface where the val-
ues of Hv are markedly lower than average with values of
Hv ≈ 30–35. This region of lower hardness occurs in the ma-
4 6 8
44.2 ± 0.5 43.2 ± 0.4 43.3 ± 0.4 41.9 ± 0.5
91.7 ± 0.6 94.8 ± 0.9 99.5 ± 0.7 –
 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76 69

Fig. 2. Color-coded contour maps showing the Vickers microhardness through the cross-sections of pure aluminum billets in the unpressed condition and after
pressing through one, two, three, four and eight passes of ECAP at room temperature using route BC : the significance of the color coding is shown at the lower
right.
70 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76
terial passing through the arc of curvature where the two
parts of the channel intersect. The presence of this region
of lower hardness near the bottom surface reduces the av-
erage hardness to Hv ≈ 40 although the remainder of the
sample generally has hardness values within the range of
Hv ≈ 40–50.
The situation after two passes is shown in the left col-
umn in Fig. 2. Again, there is a region along the lower
surface where the hardness is lower than average but in
this sample the low hardness values are in the range of
Hv ≈ 35–40 and the region is confined to within a width of
∼1 mm from the bottom surface of the billet. For the sample
pressed through three passes there is an essentially homoge-
neous distribution of hardness values with some lower val-
ues confined only to a very narrow peripheral region around
the perimeter of the billet having a maximum thickness of
<0.2 mm. The situation is similar after four and eight passes
and there is a general homogeneity in the hardness values
for these two conditions except only in a very small region,
<0.2 mm in width, immediately adjacent to the lower sur-
face.
The improvement in homogeneity with increasing num-
bers of passes is due both to a reduction in the extent of the
area at the lower surface where the hardness values are lower
than average and also to the disappearance of isolated spots of
inhomogeneity where the measured microhardness is higher
or lower than average. These spots are visible after one, two
and three passes but they are absent after pressing through
four and eight passes.
3.2.2. The Al-6061 alloy
The equivalent color-coded contour maps for the Al-6061
alloy are shown in Fig. 3: it is important to note that, for ease
in displaying the data in small incremental values of Hv, the
various colors in Figs. 2 and 3 represent different values of
Hv.
This material again exhibits excellent homogeneity in
the unpressed condition with Hv ≈ 45 throughout the cross-
section. There is a marked inhomogeneity after a single pass
with an average value of Hv ≈ 78 but with a large area, cov-
ering more than one-half of the cross-section, where the in-
dividual values of Hv are in the range of ∼65–75 and a
smaller area, primarily near the upper surface, where the
individual values of Hv are in the range of ∼90–100. As
with pure Al, the region of low Hv occurs in the vicin-
ity of the lower surface of the billet but the region is
more extensive than in the pure material. This region of
low Hv is partially removed after two passes and almost
completely removed after three passes to give a reason-
ably homogeneous microstructure. However, unlike pure
Al where the microstructure becomes homogeneous and
the hardness saturates at Hv ≈ 42–44 after four passes, the
microstructure is also homogeneous in the Al-6061 alloy
but the hardness continues to slowly increase with aver-
age values for Hv of ∼92 after three passes, ∼95 after
four passes and ∼99 after six passes. These results demon-
strate that, by comparison with pure Al, it is more difficult
to establish an equilibrium microstructure in the Al-6061
alloy.
3.3. Microstructural observations on pure aluminum
There have been extensive microstructural observations of
pure Al after ECAP [10–15] but no observations have been
undertaken to determine whether there are any differences
between the central and lower portions of the billet after a
single pass. Accordingly, these two regions were examined
separately using TEM.
Figs. 4 and 5 show representative areas and SAED patterns
after one pass near the center of the billet and very close to
the bottom surface, respectively: for both sets of photomicro-
graphs, the regions labeled (a) correspond to areas of elon-
gated grains and the regions labeled (b) correspond to areas
of reasonably equiaxed grains.
In the central region of the billet, it was estimated that
the elongated grains and the equiaxed grains each occupied
area fractions of ∼50% of the total area. For the elongated
grains shown in Fig. 4(a), the average widths and lengths
were ∼1.3 and ∼5 ␮m, respectively. For the equiaxed grains
shown in Fig. 4(b), the average grain size was ∼1.3 ␮m.
Thus, these measurements are in excellent agreement with
earlier reports, conducted on the same material, document-
ing average grain sizes of ∼1.3 ␮m [11] and ∼1.2 ␮m [15]
after four passes using route BC . Furthermore, the mea-
surements provide a clear demonstration that the equilib-
rium grain size achieved after four passes is dictated solely
by the deformation characteristics imposed on the sample
in the first pass of ECAP. Close inspection of Fig. 4(a)
reveals some partially developed but reasonably equiaxed
grains lying within the elongated grains, thereby showing
the equiaxed array develops from the elongated structure
with an average size equal to the width of the elongated
grains. It is apparent also that these grains contain large
numbers of intragranular dislocations and it is reasonable
to assume, based on earlier studies [20–23], that the grain
boundaries are in high-energy non-equilibrium configura-
tions.
The elongated grains were more prevalent in the vicin-
ity of the lower surface in Fig. 5 occupying an estimated
area fraction of ∼90% with an area fraction of only ∼10%
for the equiaxed grains. These elongated grains had aver-
age widths of ∼1.3 ␮m and lengths of ∼5 ␮m so that they
were identical in size to the elongated grains in the central
part of the specimen. It is apparent also that the diffrac-
tion spots in the SAED patterns are less broad in Fig. 5
near the bottom surface of the billet than in Fig. 4 in the
vicinity of the center of the billet so that the boundaries
introduced by ECAP have lower angles of misorientation
near the bottom surface. This observation is consistent with
the predictions of finite element analyses showing less de-
formation in the vicinity of the lower surface in ECAP
[24–26].
 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76 71

Fig. 3. Color-coded contour maps showing the Vickers microhardness through the cross-sections of an Al-6061 alloy in the unpressed condition and after
pressing through one, two, three, four and six passes of ECAP at room temperature using route BC : the significance of the color coding is shown at the lower
right.
72 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76
Fig. 4. Representative microstructures in the central part of the pure alu-
minum billet after ECAP through one pass at room temperature showing
regions of (a) elongated grains and (b) equiaxed grains.
4. Discussion
4.1. The development of homogeneity during ECAP
An important conclusion from these results is that, in
terms of the hardness distributions, pure Al and the Al-6061
alloy both develop homogeneous structures throughout the
as-pressed billets when pressed through a minimum of four
passes. However, whereas there is no significant change in
the hardness distributions in pure Al between four and eight
passes, there is a gradual increase in the average hardness val-
ues in the Al-6061 alloy up to at least six passes. This result
is consistent with an earlier report on Al–Mg alloys where
it was shown that, due to the lower rates of recovery in the
alloys, the as-pressed grain sizes were smaller than in pure
Al and it was necessary to impose a larger number of passes
in order to establish a homogeneous microstructure [27]. For
the present experiments, it was established earlier that the
equilibrium grain size of the Al-6061 alloy is ∼0.28 ␮m af-
ter ECAP [16].
Fig. 5. Representative microstructures near the bottom surface of the pure
aluminum billet after ECAP through one pass at room temperature showing
regions of (a) elongated grains and (b) equiaxed grains.
The inhomogeneities observed at the lower surfaces of the
billets are attributed to the development of a shearing zone
during ECAP as illustrated schematically in Fig. 6. In theory,
the channel within the ECAP die is bent through 90◦ and the
shear strain is applied to the sample along a sharp and well-
defined shear plane corresponding to the abrupt transition
between the two parts of the channel, as depicted in Fig. 6(a).
In practice, however, it has been shown through model ex-
periments [28,29], through finite element analyses [30–37]
and through a theoretical consideration of ECAP processing
[38] that the use of an ECAP die with a sharp corner having
an arc of curvature of Ψ = 0◦ leads to the occurrence of a
“dead zone” at this outer corner where the billet is no longer
in contact with the die wall. The development of this dead
zone is depicted in Fig. 6(b) where shearing occurs through
an angle θ defined with respect to the upper point where the
two parts of the channel intersect.
Although the problems associated with these dead zones
can be alleviated or removed through the use of dies hav-
ing movable die walls [38,39], the construction of these dies
is not easy and, from a practical point of view at least, it
 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76
Fig. 6. Schematic illustration of the principle of ECAP: (a) the theoretical model with shearing occurring along a sharp and well-defined shear plane; (b) the
situation in practice with shearing occurring through an arc denoted by the angle θ.
is more convenient to use conventional dies where the die
walls are fixed. Calculations show the value of the angle θ
subtending the dead zone depends upon both the strain hard-
ening behavior of the material and the ram speed of the press:
for example, the value of θ has been estimated as ∼51◦ for
1100 aluminum when the ram speed is ∼1 mm s−1 [35]. In
the present investigation with pure aluminum, the ram speed
was ∼7 mm s−1 and the arc of curvature machined into the
solid die was Ψ = 20◦ . It is reasonable to conclude, therefore,
that the presence of this small arc of curvature has no effect
on the pressing of aluminum because the billets move away
from the outer corner to create the dead zone. This conclu-
sion is supported by the similar results reported earlier when
pressing Al with dies having arcs of curvature of 0◦ and 20◦
[18].
4.2. A microstructural model for grain refinement in
ECAP
It is well known that processing by ECAP leads to re-
markable grain refinement in coarse-grained materials but
the general principles of this grain refinement have not been
established. A microstructural model was developed for the
refinement of grains in Armco iron when using SPD process-
ing with high-pressure torsion [40] but the model incorpo-
rates a gradually increasing refinement of the microstructure
through the continuous introduction of additional disloca-
tions during the straining process. However, a model of grad-
ually increasing refinement is not consistent with the present
observations where both the widths of the elongated grains
and the average sizes of the equiaxed grains are ∼1.3 ␮m af-
ter a single pass in ECAP and, as shown by numerous detailed
73
observations [10,11,14,15], the ultimate equiaxed grain size
in this material is also ∼1.3 ␮m up to 12 passes in ECAP.
Thus, it is important to recognize that the size of the equi-
librium substructural unit is established in the first pass of
ECAP.
It has been shown also that the ultimate equiaxed grain
sizes in ECAP are comparable to the grain sizes produced
in conventional cold-working [41]. For example, extensive
experiments on the cold-working in compression of com-
mercial purity Al at a temperature of 293 K and at strain rates
from 0.1 to 223 s−1 showed that the ultimate grain sizes were
in the range from ∼1.13 to ∼1.00 ␮m [42] which is simi-
lar to, but slightly smaller than, the grain size of ∼1.3 ␮m
reported in the present investigation on pure Al after pro-
cessing by ECAP. It is necessary, therefore, to develop a
model for grain refinement incorporating these new obser-
vations.
It is noted initially that, from the TEM observations in
Figs. 4 and 5, the area fractions of the elongated and equiaxed
grains are related to the imposed strain. The observations
show the grains tend to become more equiaxed when the
imposed strain is sufficiently large in the central region of
the billet whereas near the bottom surface, where the strain
is lower and the shearing occurs over an angular increment,
the grains are predominantly elongated.
Fig. 7 is a schematic illustration of a model for the grain
refinement occurring in the central portion of the billet for
a typical fcc metal, such as aluminum, when processed by
ECAP. The top row of Fig. 7 labeled (a) denotes the mi-
crostructures visible on the X plane after one and two passes
when using a die with Φ = 90◦ and processing route BC , the
second row labeled (b) shows the microstructures on the Y
74 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76

Fig. 7. A model for grain refinement in the central region of the billet in ECAP: (a) the substructures visible on the X plane after one and two passes of ECAP;
(b) the substructures visible on the Y plane after one and two passes of ECAP and (c) the substructures visible on the X and Y planes after four and eight passes
of ECAP; the ultimate equiaxed grain size is defined by d and the parameter ξ denotes the approximate fraction of high-angle boundaries in each substructure
based on detailed measurements on pure Al using orientation imaging microscopy [15].

plane after one and two passes, and the bottom row labeled
(c) shows the microstructures on both the X and Y planes after
totals of four and eight passes, respectively; the orientations
of the upper two rows with respect to the orthogonal X, Y and
Z directions are depicted in the small insets between the two
illustrations.
Fig. 7 also includes estimates of the fractions of bound-
aries having high-angle misorientations, ξ, for each of the
microstructures: these values of ξ are best estimates based
on a plot of the fraction of high-angle boundaries versus the
number of ECAP passes in pure aluminum [15]. It is apparent
that a higher fraction of high-angle boundaries is recorded on
 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76
the X plane for any selected number of passes and this is con-
sistent with an analysis of the shearing patterns where it was
shown that shearing extends through a larger angular incre-
ment on the X plane by comparison with the Y plane when
using route BC [43]. The values of ξ in Fig. 7(c) for the X and
Y planes are the average estimates for these two planes af-
ter four and eight passes, respectively [15]. The illustrations
in Fig. 7 are consistent with the experimental observations,
with earlier reports of the microstructures present on various
planes of sectioning when pure Al is subjected to ECAP us-
ing route BC [10,11] and with the shearing patterns predicted
theoretically [43].
In Fig. 7(a), a banded substructure is formed along the
Y-direction in the first pass where, as shown in Fig. 4(a), ap-
proximately 50% of the grains are reasonably equiaxed and
the remaining 50% are elongated: a substructure of this type
is clearly visible in an earlier report [11] and it is apparent
from OIM that a large fraction of these boundaries have low
angles of misorientation so that the structure represents an
array of elongated and equiaxed subgrains containing large
numbers of intragranular dislocations and many high-energy
non-equilibrium boundaries. The width of this banded struc-
ture measured perpendicular to the Y-axis is denoted by d.
The introduction of a second pass using route BC leads,
when viewed on the X plane, to a rotation of the banded
array through an angle of ∼27◦ with respect to the Y-axis,
the development of a new banded array lying parallel to the
Y-direction, a reduction in the fraction of elongated grains
and a gradual evolution into an equiaxed microstructure, and
a diminution in the numbers of intragranular dislocations so
that, as these dislocations become absorbed into the subgrain
walls, there is a corresponding increase in the fraction of high-
angle boundaries. Based on experimental measurements, the
fraction of high-angle boundaries in this condition is ξ ≈ 0.56
[15]. The average dimension of the minimum structural unit
introduced in this second pass is again equal to d.
Similar illustrations are presented in Fig. 7(b) for obser-
vations on the Y plane where the banded arrays lie at an angle
of ∼45◦ to the X-axis after ECAP through one pass and at
angles of ∼27◦ for the first pass and ∼45◦ for the second
pass after ECAP through two passes using route BC [43].
The predictions of the model are consistent with microstruc-
tural observations on pure Al [11] where the minimum struc-
tural dimension, d, defines the widths of the banded arrays
after one and two passes. The model assumes the subgrains
are formed initially with their longer axes oriented along the
lines of shearing introduced in ECAP and this is consistent
both with earlier observations on the ECAP processing of
polycrystalline aluminum [11] and with experiments on alu-
minum single crystals showing subgrain bands develop lying
parallel to the primary slip planes [44].
It is well-established that the appearance of the substruc-
tural arrays in pure aluminum become more equilibrated, and
essentially identical on the X, Y and Z planes, after pressing
through a total of four passes [11]. This equilibration oc-
curs through the development of shearing on multiple sets
75
of planes spread over wide angular increments on each or-
thogonal plane when processing using route BC , through the
re-arrangement of the various intersecting arrays introduced
in the different passes into a low-energy configuration and
through the absorption of many of the intragranular disloca-
tions into the subgrain boundaries. The result is illustrated in
Fig. 7(c) where there is an array of essentially equiaxed grains
having a reasonably high fraction of high-angle boundaries
after four passes so that ξ ≈ 0.56 [15]. The general appear-
ance of the microstructure remains essentially unchanged af-
ter eight (or more) passes but the OIM observations suggest
a gradual increase in the fraction of high-angle boundaries as
the imposed strain increases [15].
Contrary to the model developed earlier for Armco iron
subjected to SPD processing [40], the model in Fig. 7 ac-
counts for the initial formation of a banded structure of
elongated subgrains and the subsequent development of an
equiaxed array of grains without the introduction of any ap-
preciable change with increasing strain in the fundamental
dimensions of the smallest substructural unit. In addition, the
correlation of the measured grain size in ECAP with the grain
size produced through cold-working [41] suggests that it is
feasible to obtain preliminary information about the poten-
tial substructure introduced through ECAP by undertaking a
careful review of the relevant metal-working literature.
5. Summary and conclusions
1. Samples of pure aluminum and an Al-6061 alloy were
processed by ECAP for up to eight passes and measure-
ments of the Vickers microhardness, Hv, were recorded on
the polished cross-sections following a regular rectilinear
grid pattern. The results are presented in the form of color-
coded maps depicting the value of the local microhardness
at each point on the section.
2. The results show there is a homogeneous hardness dis-
tribution in the unpressed materials but the average hard-
ness increases by a factor of approximately 2× after a
single pass and remains reasonably constant with addi-
tional passes for pure Al but gradually increases for the
alloy.
3. The hardness distributions in both materials are inhomo-
geneous after one pass with a lower hardness in the vicinity
of the lower surface but the distribution becomes essen-
tially homogeneous with additional passes. Microstruc-
tural observations on Al show approximately equal frac-
tions of equiaxed and elongated grains in the central region
of the billet but a higher area fraction of elongated grains
(∼90%) near the lower surface.
4. The experimental results are used with earlier microstruc-
tural observations to construct a model for grain refine-
ment in ECAP. An important characteristic of this model
is that the ultimate size of the equilibrium equiaxed grains
is dictated by the width of the subgrain bands introduced
into the material in the first pass through the die.
76 C. Xu et al. / Materials Science and Engineering A 398 (2005) 66–76
Acknowledgements
This work was supported in part by a Grant-in-Aid for
Scientific Research from the Ministry of Education, Science,
Sports and Culture of Japan, in part by the Light Metals Ed-
ucational Foundation of Japan and in part by the National
Science Foundation of the United States under Grant no.
DMR-0243331.
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