Effect of Dislocation Mechanisms during Extrusion

of Nanostructured Aluminum Powder Alloy

A.M. JORGE, Jr., M.M. PERES, C.S. KIMINAMI, C. BOLFARINI, and W.J. BOTTA
Nanostructured Al-3.0Fe-0.42Cu-0.37Mn powder alloy was deformed by extrusion over a
temperature range of 375
C to 425
C, a ram speed range of 1 to 30 mm/s, and an extrusion
rate of 10:1. Flow stresses and strain rates were calculated from the experimental ram pressures
and speeds. The stressstrain-ratetemperature relationship in the extrusion of the nanostructured alloy was found to be similar to that in hot-worked conventional materials. The extrusion,
torsion, compression, and creep data of nanostructured and conventional materials, extending
over ten orders of magnitude of strain rate and over two orders of magnitude of stress, were
correlated by a hyperbolic-sine constitutive equation, because the power and exponential laws
lose linearity at high and low stresses, respectively. The hyperbolic-sine equation is widely used
to correlate the hot-working behavior of conventional materials. It was concluded that the hot
working of nanostructured powders is a thermally activated process in which the rate-controlling mechanism is the climb of edge dislocations. Microstructural changes in the consolidated alloys as a function of the extrusion conditions were investigated. An analysis was made
of the dislocation behavior in very small grains of nanostructured metal by transmission electron microscopy (TEM) and we identied a dislocation structure and the dierent ways it
appears in 40- to 100-nm Al-alloy grains. We also discuss the thermally activated propagation of
dislocations and their interactions with shear bands/grain boundaries (SBs/GBs), and dislocation loops. Microstructural features including low-angle GBs, high-angle GBs, and equilibrium
GBs and subgrain boundaries were observed. Dislocation structures under a deformation
condition were studied to investigate the microstructural evolutions, which revealed some
unique microstructural features such as dislocation tangle zones (DTZs) and dense-dislocation
walls (DDWs), and the recovery process is discussed herein.
DOI: 10.1007/s11661-009-0054-4
 The Minerals, Metals & Materials Society and ASM International 2009

I.

INTRODUCTION

NANOSTRUCTURED materials have emerged as a

new class of materials with unusual structures. In recent
years, creep and superplasticity,[1,2] cold rolling and
annealing,[3] and the quantitative understanding of the
mechanical behavior[4] of nanostructured materials have
been the subject of a number of studies.
In particular, experimental studies have focused on
grain boundary (GB) diusion creep, micrograin superplasticity, and the thermally activated propagation of
dislocations and their interactions with twin/GBs and
dislocation loops, as well as their storage in nanocrystalline grains and quantitative and mechanisms-based
constitutive models.
Despite the limited availability of data on the
mechanical behavior, especially the tensile properties,
of nanostructured materials, some generalizations can
be made regarding their deformation mechanisms. It is
likely that for the larger end of the nanoscale grain sizes,
A.M. JORGE, Jr., M.M. PERES, C.S. KIMINAMI, C. BOLFARINI,
and W.J. BOTTA, Professors, are with the Department of Materials
Engineering, UFSCar - Rod. Washington Luiz, Sao Carlos, Sao Paulo,
Brazil 13565-905. Contact e-mail: moreira@dema.ufscar.br
Manuscript submitted November 7, 2008.
Article published online October 17, 2009
3322VOLUME 40A, DECEMBER 2009

approximately 50 to 100 nm, dislocation activity dominates at test temperatures of <0.5 Tm. As the grain size
decreases, the dislocation activity apparently decreases.
The essential lack of dislocations at grain sizes below
50 nm is presumably the result of the image forces that
act on dislocations near surfaces or interfaces. The lack
of dislocations in small, conned spaces such as singlecrystal whiskers has been known for many years.[5] The
creation of new dislocations is also dicult as the grain
size reaches the lower end of the nanoscale (<10 nm).
The stresses needed to activate dislocation sources, such
as the FrankRead source, are inversely proportional to
the distance between dislocation pinning points. Because
nanoscale grains will limit the distance between such
pinning points, the stresses to activate dislocation
sources can reach the theoretical shear stress of a
dislocation-free crystal in the smallest grain sizes
(~2 nm). Thus, in the smallest grain sizes, there may
be new phenomena controlling deformation behavior. It
has been suggested that such phenomena may involve
GB sliding or grain rotation accompanied by shortrange diusion-assisted healing events.[6] A review of
these studies[14,612] shows that the data obtained by
dierent investigators are not completely consistent.
Various aspects characterizing these consistencies and
limitations are identied. It is suggested that a number
of issues need to be fully addressed in order to provide a
METALLURGICAL AND MATERIALS TRANSACTIONS A

better understanding of the deformation processes that

control the behavior of nanocrystalline materials.
Hansen and co-workers[7,8] have systematically studied the evolution of microstructures and dened microstructural features in rolled fcc metals with medium to
high stacking fault energies, such as Al and Cu.
A controversial microstructural feature in nanostructured materials processed by severe plastic deformation
techniques is nonequilibrium GB.[9] Valiev et al.[9]
dened it as a GB that contains extrinsic dislocations
that are not needed to accommodate the misorientation
across the GB. The extrinsic dislocations are usually
lattice dislocations trapped at the GB. They cause lattice
distortion near the GB and increase the GB energy.[10]
Although the nonequilibrium GB has been mentioned
by many researchers,[9,11,12] it has not been observed
directly experimentally, and this concept has been
controversial.
Previous considerations describing powder extrusion
have indicated that the relationship between ram speed
(V), pressure (P), and temperature (T) can be given by
simple equations: V = APb and P = C exp(nT).[1317]
In these equations, A and b are temperature-dependent
constants. The C is a ram-speed-dependent constant and
n is a coecient that assumes dierent values for each
metal. While these equations have reasonably wide
applications, they do not contribute much to a fundamental understanding of the deformation. In addition,
nanostructured powder extrusion has not heretofore
been considered as a thermally activated rate process.
This lack of fundamental understanding is amazing
because, in numerous aspects, the hot working of a
nanostructured powder is similar to conventional materials deformed under hot-working conditions. In fact,
there is a reasonable body of experimental evidence[16,17]
suggesting this similarity even when considering hotworking conditions with many orders of magnitude of
dierence in the strain rate. Because conventional
materials have been extensively analyzed in terms of
dislocation mechanisms, the comparison of the hot
working of such materials to that of a nanostructured
powder is important because it can suggest possible
deformation mechanisms.
Constitutive equations are used in hot working to
calculate forces in processing at set rates; T is elevated
and, with the other conditions, uctuates in practice. The
modeling of a processing stage must take into account the
nonuniform distribution of e, e_ ; and T and their variation
with time; it may need several constitutive functions,
depending on the complexity of the ow curves.
One 0of



the constitutive equations is the power law e_ A1 rn ;
which breaks down at high stress, i.e., the stress
exponent n varies with e_ : In the past, researchers studying
hot
working
favored
the
exponential
law
e_ A2 expbr
expDH=RT but it breaks down at
high T below 1 s1. A function that includes both
equations in the limits was introduced in the 1960s:[1831]
A3 sinharn e_ expDH=RT Z

1

where A3 (A1, A2), a (b/n), n, n, b, and DH

(R = 8.31 J mol1 K1) are material constants. The
METALLURGICAL AND MATERIALS TRANSACTIONS A

ZenerHollomon parameter embraces the two control

variables e_ and T in the hot-working process. The stress
multiplier a is an additional adjustable constant that
brings ar into the correct range to make constant T
curves in log e_ vs log sinh (ar) plots linear and parallel.
As a increases, n decreases almost inversely and the
slope of the Arrhenius plot (log sinh arvs l/T) rises
almost linearly. The result is the activation energy DH
(=2.3 R n slope) rises or falls to a stable value. Note that
it is preferable to compare the DH and n values of
dierent alloys of a given metal at a xed a; generally
n n, although it does occur at a certain a.
This equation was proposed for the correlations of
creep data by Garofalo,[32] and was subsequently modied and applied to hot torsion by Sellars and Tegart.[33]
The objectives of the present work are the following:
(1) to analyze the hot extrusion of nanostructured
aluminum alloy powder from the standpoint of thermally activated deformation mechanisms in comparison
with the mechanisms operating in conventional materials; (2) to study the microstructural features and dislocation congurations in a nanostructured Al-powder
alloy processed by extrusion; and (3) to investigate the
microstructural evolutions through transmission electron microscopy (TEM) observations of dislocation
structures during hot-working conditions.

II.

MATERIALS AND METHODS

Rapidly solidied aluminum alloy powder with a

nominal composition of Al-3.0Fe-0.42Cu-0.37Mn
(wt pct) was prepared using argon gas atomization.
A nanostructured aluminum alloy powder with an
average grain size of 25 nm was obtained. Cylindrical
preforms of the nanostructured powder were prepared by
cold pressing and then used for consolidation processing
with a relative density of approximately 0.96 and an
initial diameter of 26.2 mm. The preforms were then
consolidated into 7.9-mm-diameter bars of bulk material
by hot extrusion at three dierent temperatures (375
C,
400
C, and 425
C), an extrusion ratio of 10:1, and ram
speeds of 1, 15, and 30 mm/s. Microstructural observations were carried out by TEM using a PHILIPS*
*PHILIPS Microscopes are now owned by FEI Company,
Hillsboro, OR.

CM-120 microscope. Thin foils for TEM observation

were prepared by ion milling.
To compare ow stress extrusion data with any other
kind of deformation test data, we used the wellestablished methodology described in the literature[3437]
to correct the homogeneous deformation, the sliding
resistance of the billet due to friction, and the redundant
work eects. This procedure is necessary because the
extrusion pressure does not represent the true ow stress
of the material; in addition, the steady-state ow
stress acting during extrusion cannot be determined
from the extrusion pressure. Therefore, we calculated

VOLUME 40A, DECEMBER 20093323

the equivalent stress acting during extrusion as follows.[3437]

d
e

(a) The true stress can be calculated by the following

equation:



r
P
h

r

P
 t
Pf


r

P 
r

r

is the mean true stress, Ph is the pressure

where r
to the homogeneous deformation, Pf is the pressure due to the friction, Pr is the pressure to the
redundant work, and Pt is the total pressure acting
during the extrusion process (Pt = Ph + Pa + Pr).
r can be
(b) The homogeneous deformation Ph =

calculated by the following equation:

Ph Wh

lZ
n ER

rde
0

where Wh is the work of the homogeneous deformation by unit volume, ER is the extrusion ratio,
r is the ow stress, and e is the strain. However,
for large strain values in hot-working processes, Ph
can be expressed by

ln ER
Ph r

is the mean true stress; i.e.,
where r
Ph
ln ER cte


r



(c) The friction Pf =

r can be calculated by the following equation:
Pf
1; 5 ln ERfexp4lL=D0   1g


r

is the mean true stress, ER is the extrusion
where r
ratio, l is the friction, L is the extruded length
until the cone, and D0 is the container diameter.
The l can be calculated as
l

D0 dp
4p dx

where D0 is container diameter, p is the instantaneous pressure, and x is the axial distance along
the container.
r can be calculated by
(d) The redundant work Pr =

the following equation:
Pr 1:5Ph

 ln ER


r
rc
where rc is the interpolated ow stress obtained from
data of hot compression tests in the extruded alloy.
Equations [2] and [3] were used to estimate the mean
equivalent strain and mean strain rate, respectively.[38]
3324VOLUME 40A, DECEMBER 2009

dl
)
e
l

Z
0

dl
l
ln
l
l0


6VD2 tan u
DC

e
3 C 3  2 ln
DE
DC  DE

2

3

where l0 is the initial length, l is the instantaneous length,

V is the ram speed, DC is the container diameter, DE is
the extrusion diameter, and u is the semiangle of the
conical die or dead zone metal zone.
A minimum square method was applied to t the
experimental data to rate and constitutive equations
(activation energy determination, nonlinear equation
t). The program developed for this work consists of
three algorithms to solve equation systems applying the
methods of NewtonRaphson, Steepest Descent, and
Marquardt. This software program is a variant of the
VA05A and MB11A routines of the Harwel Subroutine
library (available in FORTRAN) (Science & Technology
Facilities Council (STFC), Oxfordshire, UK), used in
mainframe computers adapted to personal computers.

III.

RESULTS AND DISCUSSION

In order to evaluate the stress dependence of the

strain rate under the extrusion conditions of nanostructured powders, and to compare it to that of conventional materials processed in similar conditions, the
extrusion data were analyzed according to Eq. [1]. To
determine the activation energy, we solved Eq. [1] using
a method described in the methodology, but for
discussion we are using the graphical methodology
similar to that proposed by Uvira and Jonas.[39]
Figure 1 plots log e_ vs log sinh (ar) using a value of
47.83 9 103 MPa1 for a. With this parameter, it is quite
obvious that log e_ is a function of log sinh (ar) and,
therefore, the extrusion of nanostructured powder data
are very well described by the hyperbolic sine equation. A
constant slope of 3.6 is obtained over the whole range of
the stress. The fact that a constant value of a was used in
the entire range of data and that the slope n is independent of temperature supports Sellars and Tegarts[33] view
that a and n are largely independent of temperature.
From this discussion of the stressstrain-rate relationship for the hot extrusion of a nanostructured
powder, it appears that well-established Eq. [1], using
similar material constants, can be used to satisfactorily
describe such phenomena.
From the standpoint of the response of the material,
therefore, the processes discussed earlier appear to be
inherently similar. As will be seen later, the deformation
mechanisms operating during the hot working of
conventional materials are indeed similar, but before
elaborating on this theme, a comparison will be made of
the stressstrain-rate relationship for the creep and hot
extrusion of conventional materials and nanostructured
powders.
Figure 1(b) shows data from the literature on the
strain rate vs sinh (ar) in the case of hot extrusion[40] and
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 1(a) Hot extrusion data for nanostructured Al-3.0Fe-0.42Cu0.37Mn powder alloy, showing applicability of the hyperbolic sine
law (Eq. [1]). (b) Hot extrusion data from (a) plotted together with
hot extrusion data from the literature (commercial-purity aluminum,
99.73Al-0.21Fe-0.06Si)[40] and creep data from the literature (superpurity aluminum, 99.9945 pct Al),[41] showing the compatibility of
hot-working data obtained at high strain rates and strains from both
conventional material and nanostructured powders with those of
creep obtained at low strain rates and strains. Data plotted according to Eq. [1].

aluminum creep[41] plotted with the experimental extrusion data obtained in the present work. The similarity of
the stress dependence of the extrusion strain rate to that
of extrusion and creep of conventional material is
somewhat surprising, mainly with respect to creep,
because the extrusion strain rates are several orders of
magnitude higher than those found in creep. However,
this observation conrms our suggestion that the hot
extrusion of nanostructured powders may be considered
an extension of any other hot-working process.
The data shown in Figure 1(b) extend over a 1010-fold
range of strain rates. Bearing in mind the large range of
strain rates and taking due note of the dierences in the
purity of the materials, the congruence of the hot-working
data to the creep equations is exceptionally close, resulting in similar values of the equation constants. However,
there is a slight dierence in the slope n between the data
reported in the literature and our experimental data. For
creep of the high-purity aluminum, n = 4.8, and for the
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 2(a) Hot extrusion data for nanostructured Al-3.0Fe-0.42Cu0.37Mn powder alloy, hot extrusion data from literature (commercial-purity aluminum, 99.73Al-0.21Fe-0.06Si),[40] and creep data from
the literature (super-pure aluminum, 99.9945 pct Al),[41] plotted to
illustrate the dierence in the slope n of all the materials,
Z e_
expDH=RT: (b) Plot of sinh(ar) at a constant strain rate as a
function of 1/T, from which the slope is used to determine the hotworking activation energy.

extrusion of commercial-purity material, n = 4.1,

whereas the extrusion of nanostructured Al powders
shows n = 3.6. These dierences in the values of n are
illustrated clearly in Figure 2(a), which plots log
ZZ e_
expDH=RTvs log(sinh(ar)). As observed by
other authors,[4244] this range in stress exponent values
(3.6 to 5) corresponds to dislocation climb. Moreover, we
did not obtain a remarkable stress drop on the stressstrain curves. It is well known that the stress drop is
related to the GB sliding, while the slip lines represent the
dislocation slip.[45]
The dissimilarity in the value of n is also in conformity
with hot-working observations of conventional materials of dierent purities and deformation mechanisms.
The hyperbolic sine exponent n (which is equivalent to
the power law exponent at low stresses) has been shown
in creep studies to be higher for pure metal,[46] although
this eect is not expected to be very signicant. The
incorrect choice of the same value of a for materials of
dierent purities is more likely to justify the dissimilarity.
VOLUME 40A, DECEMBER 20093325

It might be expected that had a dierent, appropriate a

been used for each material, as required, the values of n
would have been more closely related.
Comparisons can be made of the temperature dependence of the strain rate in the hot extrusion of
nanostructured powders against other types of hotworking processes in conventional materials by comparing the values of experimental activation energies.
However, due to the nature of hot-working tests. The
activation energies for all the data obtained here were
calculated according to the methodology proposed by
Uvira and Jonas,[39] solving Eq. [1] as described under
Section II.
Graphically, the Uvira and Jonas method considers
the stressstrain-rate relationship in Eq. [1] as follows:

 
 

d log e_
d log fr
d log e_
DH
4



1
d log fr T
dT1
dT
2; 3R
e_
r

Figure 3 shows that the stress increases with an

increasing strain rate and a decreasing deformation
temperature. As can be seen, the maximum stress
increases with an increasing strain rate and a decreasing
deformation temperature. In a general way, the maximum stress is followed by steady-state ow behavior.
The observed behavior has been related to the occurrence of dynamic recovery. Furthermore, the related
ow behavior can be attributed to any microstructural
instability, such as the dynamic recovery, texture formation, pinning of dislocation by precipitates, or
dissolution of precipitates.
In this work, precipitates were used to control the
grain growth. The precipitation behavior of the alloy
studied in this work was analyzed by Jorge, Jr. et al.[48]
Initially, the alloy was precipitate rich. When the
temperature was increased, the results obtained by the
authors indicated both precipitate coarsening and
dynamic dissolution. In fact, as was observed by Jorge,
Jr. et al.,[48] at high temperatures, the majority of the
present precipitates are dissolved in the Al matrix. These
solutes assist in pinning the dislocation, therefore
resulting in the work hardening of the alloy. However,
the rate of work hardening is balanced by the worksoftening eects due to the dynamic recovery. Decreasing the stress level by reducing the strain rates is related
to a stronger eect of the dynamic recovery phenomenon during strain application.
As is seen at the lowest deformation temperature
(375
C) and at the highest strain rate (29.3 s1), the
work hardening is unable to equilibrate the work
softening. The latter results in a continuous softening
and, thus, a decreasing of the ow stress during
deformation. Flow softening is a common characteristic of true-stresstrue-strain curves of many alloys
deformed at elevated temperatures. In the particular
case of this work, it is believed that the dynamic
recovery and coarsening of existing precipitates along
with local ow near the boundaries can be responsible
for the softening at high temperature.
However, by deformation at 375
C with a strain
rate of 29.3 s1, the temperature and time by themselves appear to be inadequate for the dissolution of

where each of the terms on the left side of the equation

is obtained from direct experimental measurements
(Figures 1(b) and 2(b), respectively). Figure 2(b) shows
the stress dependence on the temperature at a constant
strain rate from which the slope is used to determine the
activation energy for hot-working processes.
Table I presents the results of the activation energies
for hot extrusion data for the nanostructured Al-3.0Fe0.42Cu-0.37Mn powder alloy, as well as hot extrusion[40]
and creep data[41] from the literature, which summarizes
the material constants n, a, DH, and A3 for the set of
data considered here. It is evident that the constants of
Eq. [1] have similar values for the three materials in hot
extrusion and in creep. This also supports the argument
that the hot extrusion of nanostructured powders and
hot-working processes in general are thermally activated
deformation processes similar to high-temperature creep
and the hot extrusion of conventional materials, in spite
of the dierences in the orders of magnitude of their
strain rates.
For the alloys tested in stable conditions, Eq. [1]
results in DH values that are close to, but invariably
slightly higher than, the activation energy for selfdiusion in Al (143 kJ mol1).[47]
Table I.
Temperature
(
C)
320
376
445
490
555
204
260
371
482
593
375
400
425

Summary of Constants n, a, DH, and A3 for Hot Extrusion Data for Nanostructured Aluminum Powder Alloy
and Hot Extrusion and Creep Data from Literature
n
4,0
4,0
4,0
4,0
4,0
4,8
4,8
4,8
4,8
4,8
3.6
3.6
3.6

a (9103 MPa1)
43.51
43.51
43.51
43.51
43.51
44.96
44.96
44.96
44.96
44.96
47.83
47.83
47.83

3326VOLUME 40A, DECEMBER 2009

DH (kJ/mol)
156.5
156.5
156.5
156.5
156.5
156.1
156.1
156.1
156.1
156.1
164.8
164.8
164.8

Remarks

A3
0.11
0.96
1.33
1.47
1.79
1.03
0.43
0.63
0.87
1.08
3.27
4.00
3.64

9
9
9
9
9
9
9
9
9
9
9
9
9

10

10
1010
1010
1010
1010
1012
1012
1012
1012
1012
1011
1011
1011

[40]

extrusion: commercial-purity aluminum

(99.73 pct Al)

creep:[41] high-purity aluminum (99.9945 pct Al)

extrusion (present work) (Al-3.0Fe-0.42Cu-0.37Mn)

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 3Flow stress behavior of the alloy studied in this work, at

(a) 0.98 s1, (b) 14.7 s1, and (c) 29.3 s1.

precipitates, and this may lead to an increase in the ow

stress. In this situation, the presence of precipitates
hinders dislocation glides, raising the ow stress, but the
ne precipitates are a more eective source of strengthMETALLURGICAL AND MATERIALS TRANSACTIONS A

ening. By continuing the deformation, due to the

presence of such ne precipitates, the dislocation density
increases, so pipe diusion increases the kinetics of the
coarsening of the precipitates. The latter may increase
the kinetics of recovery. Therefore, the decrease in the
ow stress beyond the maximum stress under this
condition (lowest temperatures and highest strain rates)
is related to the dynamic coarsening and morphological
changes of precipitates from coherent to noncoherent.
In the other conditions, due to the higher temperature
or lowest strain rates (longer time), the atomic diusion
increases and the growth rate of precipitates increase
during deformation. This may lead to a signicant
decrease in the rate of work softening compared to the
aforementioned condition, due to the larger size of the
precipitates. It is believed that above the temperature
range of morphological changes in precipitates, the
work-hardeningwork-softening balance is achieved.
Figure 2(b) shows the variation in the maximum
stress as a function of the inverse temperature at
dierent strain rates. This clearly indicates that the
strengthening eect of the particle-dislocation interaction gradually decreases with increasing temperature
and decreasing strain rate. This, in turn, is easily
explained by the coarsening and, at a higher temperature and longer times, the dissolution of precipitates. In
fact, with the temperature increasing or the strain rate
decreasing, due to the coarser particle size and larger
spacing, the precipitates have a minor strengthening
eect. In addition, the solute level is also low in this
condition. In the present study, the recovery is the
controlling mechanism due to the coarsening of the
precipitates and the removal of solute elements from the
matrix. The calculated activation energy also conrms
the activity of this mechanism.
In this context, as can be noted in Table I, the value of
the constant n is strongly inuenced by the presence of
precipitates or alloying elements, i.e., with the increase
of alloying elements, n is severely decreased, when
compared with the changes in a and DH. This, in turn,
could mask the physical interpretation of the n value.
The values of DH listed in Table I indicate that the
hot extrusion of nanostructured aluminum powder alloy
is diusion controlled, as in the case of conventional
materials. The experimentally observed stress dependence and the evidence of the microstructural/substructural changes taking place during extrusion, as will be
discussed later, with the stress exponent value (n)
obtained in this work (3.6) indicate that the ratecontrolling mechanism is the climb of edge dislocations,
as in the case of the hot working of conventional
materials.
Based on the values of a, DH, and A3 presented in
Table I, Figure 4 graphically illustrates the compatibility of the hot extrusion data of nanostructured powders
and the hot extrusion and creep of conventional
materials. This gure is similar to Figure 2(a), except
that Z is divided by A3. Dividing Z, the Zener
Hollomon parameter, by A3 removes the eect of the
purity dierences among the three materials.
Thus, experimental data from the hot extrusion of
nanostructured powders and the hot extrusion and creep
VOLUME 40A, DECEMBER 20093327

of conventional materials extending over a 1010-fold

range in strain rates and a hundredfold range in stress
can be represented by the hyperbolic-sine constitutive
equation, Eq. [1], using the same material constants with
little data scattering. The slope of this plot is 4.52.
Figure 1 shows the dependence of the extrusion
steady-state stress of the strain rate on the test temperature calculated from the experimental data. As in the
steady-state hot working of conventional materials, the
ow stress for the steady-state hot extrusion of the
nanostructured Al alloy decreases with an increase in
temperature and a decrease in strain rate. As discussed

Fig. 4Graphic illustration based on the values of a, DH, and A3

presented in Table I, showing the compatibility of hot extrusion data
of nanostructured powders and hot extrusion and creep of conventional materials.

earlier, this can be attributed not only to the increase in

the number of thermally activated events taking place
per unit strain but also to modications in the dislocation arrangement caused by deformation at the higher
temperatures or strain rate reciprocals.
The TEM micrographs in Figures 5(a) and 6(a)
indicate that individual grains were produced with sizes
ranging from less than 100 nm to a few hundred
nanometers, separated by high-angle GBs. Most of the
grains were heavily strained and contained a high
density of dislocations. The corresponding electron
diraction pattern in Figure 5(a) shows diraction
rings, indicating a polycrystalline structure and the
small grain dimension. Figure 5(b) (zoomed in
Figure 5(c)) shows one of the mechanisms for dislocation multiplication under stress, which can be observed
on a dislocation segment pinned at its ends, in which the
white arrowhead denotes the dislocation lines (DLs)
interacting with SBs.
Figure 6 shows TEM micrographs of dierent regions
of the specimen. A number of ne structures were
observed inside the grains. As indicated by the white
arrowhead in Figure 6(a) (and zoomed in Figures 6(b)
and (c)), an array of dislocations piled up along a
crystalline plane. Consequently, three subgrains
(denoted by 3) with a low misorientation were produced.
This grain also shows a low-angle GB, which is marked
by four stars in Figure 6(b). The low-angle GB was
formed by the accumulation of dislocations. This is clear
evidence of a recovery process in which dislocations
migrate to form a strain-free subgrain boundary. The
dislocation cell structure was also observed in subgrains
2 and 4 in Figure 6(a). Dislocation tangling was
frequently observed in the interior of grains, as indicated

Fig. 5TEM micrographs showing (a) nanostructured Al-alloy produced by hot extrusion process and corresponding electron diraction
pattern (EDP), showing fcc-Al diraction rings, indicating a polycrystalline structure and small grain dimension; (b) and (c) one of the mechanisms for dislocation multiplication under stress, which is visible on a dislocation segment pinned at its ends, while the double white arrowhead
(c) denotes the DLs interacting with SBs, indicated by black lines). Specimen extruded at 425
C and 29.3 s1 (magnications (a) and (b) 166,000
times).
3328VOLUME 40A, DECEMBER 2009

METALLURGICAL AND MATERIALS TRANSACTIONS A

plotted in Figure 1 are the result not only of structural

modications but also of changes in the thermally
activated events due to the strain.

IV.

SUMMARY AND CONCLUSIONS

The following conclusions can be drawn from this

study.

Fig. 6(a) through (d) TEM micrographs showing ne deformation

structures. Numbers 1 through 4 denote subgrains; the white arrowhead (a) points to an array of dislocations piling up along a crystalline plane; the four stars (b) mark a low-angle GB; the white circle
(a) marks a DTZ; the white square (a) marks a transition from DTZ
to dislocation cells; (d) shows parallelogram-shaped subgrains with a
size of approximately 22 nm are delineated clearly by the DDWs.
Specimen extruded at 425
C and 29.3 s1 (magnication (a) 166,000
times).

by a white circle in Figure 6(a), in which the grain is

heavily strained. We shall refer to such a region as a
dislocation tangle zone (DTZ). The white square marks
a transition from a DTZ to dislocation cells.
Figure 6(d) shows another example of subgrains
generated from larger grains. The parallelogram-shaped
subgrains with a size of approximately 22 nm are
delineated clearly by the dense dislocation walls
(DDWs). These subgrains are clearly inside a larger
grain and are isolated from other subgrains. The
dislocation density is higher inside than outside the
subgrains.
The similarities between the hot extrusion of a
nanostructured Al alloy and the hot working of conventional materials in terms of the interdependence of
stress, strain rate, and temperature in rate-controlling
mechanisms will now be discussed, as well the eect of
the substructure on ow stress.
The straight-line plots illustrated in Figure 1 and all
results discussed in previous sections show that in the
extrusion of the nanostructured Al alloy, the stress
dependence of the strain rate can be given by a
hyperbolic sine function, as is already observed in the
hot working of conventional materials. There is also a
similarity in the temperature dependence of the strain
rate in nanostructured and conventional material under
hot-working conditions, in that both can be expressed
by an Arrhenius law.
When the imposed temperature is raised or the
imposed strain rate is decreased, the enhanced mobility
of the dislocation leads to a greater rate of annihilation
and a lower equilibrium dislocation density. Figures 5
and 6 show that the changes in the substructure
geometry depend on thermally activated events that
only can be produced by straining, as is the case in
conventional materials. Because the stress required to
maintain a steady-state deformation is also a function of
the temperature and strain rate, it follows that there is a
denite relationship between the stress and the substructure geometry. Furthermore, the ow stresses

METALLURGICAL AND MATERIALS TRANSACTIONS A

1. The analysis of the experimental results of this

work for nanostructured powders compared with
others from the literature for conventional materials
indicated that the hot extrusion data of nanostructured powder can be expressed by well-known
hyperbolic-sine constitutive equations using similar
material constants. This observation is valid despite
the dierences in the orders of magnitude of the
strain rates used in other hot-working tests.
2. The experimental activation energy for the hot
extrusion of the nanostructured aluminum powder
alloy was similar to those for the hot extrusion and
high-temperature creep of conventional materials
and for self-diusion. This indicates that the
rate-controlling mechanism in the hot extrusion of
nanostructured aluminum powder alloy is diusion
controlled. Further comparison of hot-working data
from the literature with theoretical stress laws for
diusion-controlled deformation mechanisms indicates that the rate-controlling mechanism is the
climb of edge dislocations.
3. The evolution of the substructure observed in this
work was similar to the substructures formed during the hot working of conventional materials, indicating that considerable dynamic recovery had
occurred.

ACKNOWLEDGMENTS
The authors acknowledge the nancial support of
the Fundacao de Amparo a` Pesquisa do Estado de
Sao Paulo (FAPESP) and the Conselho Nacional de
Desenvolvimento Cient co e Tecnologico (CNPq).

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