Acta metall, mater. Vol. 42, No. 7, pp.

2467-2475, 1994
Copyright 1994ElsevierScienceLtd
Pergamon 0956-7151(94)E0006-3 Printed in Great Britain.All rights reserved
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DEFORMATION BEHAVIOUR OF ULTRA-FINE-GRAINED

COPPER
R. Z. VALIEVlt, E. V. KOZLOV z, YU. F. IVANOV z, J. LIANI~, A. A. NAZAROVlf and
B. BAUDELET 1
~G6niePhysique et M6canique des Mat6riaux, Unit6 Associ6e au CNRS, Institut National Polytechnique
de Grenoble, ENSPG, BP 46, 38402, Saint Martin d'H6res, France and 2Department of Physics,
Construction and Engineering Institute, 634050 Tomsk, Russia

(Received 3 June 1993; in revised form 27 October 1993)

Abstract--Mechanical behaviour and structural changes, such as the evolution of grain and dislocation
structures and the formation of slip lines and grain-boundary-sliding traces, of a submicron-grained
(SMG) copper during room-temperature compression have been studied. It is suggested that the
absorption of dislocations into grain boundaries (GBs) is due to the migration and sliding of some highly
non-equilibrium GBs during the deformation process and is influenced by high level internal stresses.
From this point of view, the unusual behaviour of SMG copper, in particular, the high yielding and flow
stresses, the absence of strain hardening, high plasticity and low strain rate sensitivity, are explained.
Analogies of the mechanical behaviour of SMG copper with mechanical properties of metallic materials
at large plastic strains in stage IV are discussed.

1. INTRODUCTION non-equilibrium state to an equilibrium state during

In the last few years materials with ultra-fine grain
(UFG) structures (both nano- and submicro-crystals)
have attracted a growing interest of research.
Changes of usually structure-insensitive parameters
[1, 2], e.g. elastic moduli, Curie and Debye tempera-
tures, saturation magnetization, etc., in these ma-
terials have encouraged expectations of their unusual
properties. Indeed, many enhanced mechanical
properties including high strength and ductility, su-
perplasticity and damping have been revealed by
studies of different U F G materials.
However, regularities of their deformation be-
haviour, structural changes and deformation mech-
anisms are still a matter of controversy. For example,
some studies have shown a material-softening effect
with decreasing grain size to nanoscale, giving a
negative coefficient to the Hall-Petch (H-P) relation
[3, 4], whereas normal H - P relations with positive
slopes have been found in others [5-7]. The reason for
this difference is not yet fully clear. Nevertheless,
recent studies [8-11] have shown that an additional
annealing can lead to changes in the H - P relation
slope without changing grain size. It has also been
observed that GB conditions can recover from a
"t'On leave from the Institute for Metals Superplasticity
Problems, Russian Academy of Sciences, 39 Khalturina,
450001 Ufa, Russia.
*On leave from the Department of Metal Materials Engin-
eering, Jilin University of Technology, Changchun
130025, P.R. China.
annealing [2, 9]; this is obviously an important feature
for the strength of those materials. Another unclear
but rather important question is on the characteristics
of the strain hardening effect in U F G materials.
Certain problems exist due to the fact that most
data on mechanical properties of U F G materials
are from hardness measurements. Meanwhile,
tensile tests of typical nanocrystalline materials
have shown that the samples are brittle [12] and
that the measured strengths appear to be affected
by flaws and do not represent intrinsic mechanical
behaviour [10]. Furthermore, deformation mechan-
isms in U F G materials have not been well under-
stood. All these uncertainties require further
investigations into the deformation behaviour of
these materials.
For this purpose, studies of U F G metallic ma-
terials prepared by severe plastic deformation are of
great interest, for the method of severe plastic defor-
mation is capable of providing bulk samples having
grain sizes below 0.1 # m and free of residual porosity,
which are suitable for mechanical testing including
the superplasticity study [2, 13]. Recent studies on the
H - P relations in these materials [9, 1l] have shown
that they behave in a rather similar way to typical
nanocrystalline materials [10]. It should also be
pointed out that studies of plastic deformation of
U F G materials can also aid the prediction of the
behaviour of materials during high plastic defor-
mation in stage IV [14, 15]. All the reasons mentioned
above initiated the present study of the mechanical
behaviour, structural changes and deformation

2467
2468 VALIEV et al.: D E F O R M A T I O N BEHAVIOUR OF U F G COPPER
mechanisms of copper with submicron grain struc-
tures produced by severe plastic deformation.
2. EXPERIMENTAL MATERIAL AND PROCEDURES
Copper samplers of purity 99.98 % were used in the
experiments. The submicron grained structure was
produced by using equal-channel angular (ECA)
pressing technique at room temperature without any
intermediate annealing [16, 17]. During ECA press-
ing, samples with initial dimensions of 14 14
60 mm 3 and a grain size of approx. 300 #m, were
subjected to shear deformation by pressing through
two channels of equal cross-section intersecting at an
angle of 7z/2. In this procedure, a pure homogeneous
shear is localized at the intersection of the two
channels and the as-deformed dimensions are identi-
cal to the initial ones so that repetitive pressings can
be continued up to the required level of plastic
straining. In the present experiments, the material
was deformed continuously to an equivalent true
plastic strain approximately equal to 4.
Specimens of 4 4 6 mm 3 for compression were
cut from the pressed material with the compression
direction being parallel with the pressing axis. Com-
pression tests were carried out at room temperature
using an Instron type testing machine operating at a
constant rate of anvils displacement. The initial strain
rate was 1.4 x 10 -3 s -~.
Microstructures of the specimens were studied by
TEM using both thin foils and high resolution carbon
replicas shadowed by platinum under a given angle
(20). Replicas were obtained from specimen surfaces
parallel with the compression direction. Shadowing
of the replicas allowed for measurements of the
height of surface steps formed as a result of sliding
[18, 19]. To estimate the strain component due to
grain boundary sliding (Egbs) relative to the total
deformation (Etot), we used the following equation
[18, 20, 21].
Egbd ~- khn
where k is a constant, h is the average value of step
heights and n is the average number of displacements
per unit length. In accordance with experiments on
fine-grain materials [18, 20], k has been taken equal to
1.5. Thin foils were cut normal to the compression
axis and were prepared using conventional electro-
chemical jet-thinning method, as described in Ref.
[16]. Two electron microscopes, EM-125K and TEM
2000CX, were used for the structural studies. Struc-
tural parameters (grain sizes and dislocation den-
sities) were estimated using the linear intercept
technique. Dislocation densities in the specimens
were close to the maximum density measurable by
TEM. For this reason the weak beam technique [22]
was used to obtain a higher resolution and a better
contrast. More than 200 measurements on several
negatives have been made and the accidental errors
did not exceed 10%.
3. EXPERIMENTAL RESULTS
3.1. Mechanical behaviour
Figure 1 presents a true flow stress-strain curve in
compression of a copper specimen with a mean grain
size of 210 nm (curve 1). The test was performed at
room temperature with an initial strain rate of
1.4 10 -3 s -~. To compare with curve 1, the flow
stress-strain curve for a copper specimen of the same
composition but with a grain size of 30 # m is also
shown in the figure (curve 2). It is seen that the flow
stress dependence on compression strain of S M G
copper has a different shape from that of conven-
tional copper materials. Typical features of defor-
mation behaviour of the SMG copper are as follows:
high yielding stress equal to 390 MPa, remarkable
strain hardening effect within a narrow strain range
(approx. 5%) at the initial stage of deformation, and
followed by a long stage of deformation almost with
no hardening. The flow stress in the last stage is as
high as 500 MPa. After straining to about 50% a
small hardening was observed. At the same time, the
ductility of SMG copper is high. Specimens did not
fracture even after the maximum strain of 83%
applied in the experiments.
3.2. Microstructure of as-prepared samples
A micrograph of the typical structure of the S M G
copper just after preparation is shown in Fig. 2(a).
The average grain size is 210 nm and the distribution
of grain size is similar to a log-normal function. In
this micrograph, three types of grains can be distin-
guished. The small grains of 50-200 nm are almost
free of dislocations. The grains of 100-200 nm have
chaotically distributed dislocations. The large grains
of 100-500 nm contain sub-boundaries. The fractions
of these grains in the structure were approx. 15, 37
and 48% for the three types, respectively. The aver-
age dislocation density in the as-prepared state was
determined to be approx. 5 1014m -2. It should be
noted, however, that this is the lower limit of the
density, since there might be some rearrangement of
dislocations during the preparation of foils due to
high internal stresses.
600
1
~ , L J. ak /.
500
400
300
~ _ _ - - 2- .
200
100
0
0 0.1 0.2 0.3 0.4 0.5
E
Fig. 1. True stress-strain curves of room-temperature com-
pression tests for copper samples with mean grain sizes of
210nm (1) and 30pm (2), ~ = 1.4 x 10-3s -l.
 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER 2469

Fig. 2. (a) Transmission electron micrograph of a typical SMG copper microstructure in initial as-prepared
state; (b) diffraction pattern corresponding to this structure taken from an area of 0.5 pm 2.

Another important feature in the original state of
the samples is the presence of extinction contours
inside many grains, indicating high internal stresses
[23]. Extinction contours are often observed in dislo-
cation-free grains. This suggests that the sources of
the high internal stresses are in grain boundaries.
Such internal stresses have been observed by TEM
and X-ray techniques in a number of U F G materials
produced by severe plastic deformation [2, 9, 11].
The grain structures of the specimens are of gran-
ular type, i.e. the grain boundaries are mainly high-
angle ones, as evident from a selected area electron
diffraction pattern shown in Fig. 2(b). The pattern
was taken from an area of 0.5/~m 2 and contains
numerous spots arranged in circles like those from
typical polycrystals [24]. Moreover, recent TEM
examinations of SMG samples using micro-diffrac-
tion analysis with the electron beam focused individ-
ually on each grain provided evidences for high-angle
misorientations between neighbouring grains [25].
Recently, the formation of such a granular structure
in Ni3AI after severe plastic deformation followed by

AM 42i7--S
2470 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER

350 density was not changed during further deformation.

The majority of grain boundaries also maintained
their complex contrast, i.e. remained in highly non-
300 Theoretical Prediction equilibrium states.
Q=7OKJ/mol, Dgb0=2.35E-5 J 3.3.2. Surface studies. Deformation relieves
formed on pre-polished surfaces during straining
E were revealed by high-resolution replicas. Studies on
= 250 07KJ/mol
these replicas gave the following information.
Slip lines appeared after deforming to 25%. Only
one slip system operated in each grain. Slip lines
200
crossed the whole grain from boundary to boundary
Cu, da=210nm; e x p .
and distributed uniformly within one grain. The
T=293K resolution of replicas was about 2 nm. Therefore,
150 i i i J i J

100 200 300 400 500 600 700

Time (S)
Fig. 3. Experimental values of the mean grain size in SMG
copper after different strains ( i ) and theoretical predictions
for grain growth calculated using equation (8): curve I with
Qb = 107 kJ/mol; curve 2 with Qb = 70 kJ/mol.

annealing at temperatures above 523 K has been

reported [11]. In copper, due to a lower melting
temperature, the granular structure is formed without
subsequent annealing, directly during deformation,
as also observed in aluminium-magnesium alloys [9].
Most grain boundaries are highly non-equilibrium.
Only approx. 10% of GBs have banded diffraction
contrast typical for boundaries in well annealed
materials. In general, the images of GBs are charac-
terized by specific spread or more complex contrast
[9, 11, 13].

3.3. Structural changes during deformation

3.3.1. Grain and dislocation structures. Studies on
structures of samples have shown that grain sizes
increased during deformation. Static grain growth in
this material has only been observed during annealing
at 200C [16]. Therefore, the grain growth observed
in this case was caused by deformation. The average
grain size (taking account of the cross-section in-
crease due to compression) is plotted in Fig. 3 as a
function of strain. Some grains grew up to
600-900 nm after straining to 53-80%.
The distribution of grains of the three types is also
changed with deformation. The percentage of dislo-
cation-free grains remained unchanged at 10-15%.
The number of grains with chaotically distributed
dislocations increased to 50-60%. Typical examples
of the structures after deformation to 29, 53 and 83%
are presented in Fig. 4(a), (b) and (c), respectively. It
is seen that internal stresses remained high, as
suggested by the high density extinction contours in
many grains. It is noted that after some deformation
(E =0.05) the average dislocation density slightly
increased to 10 ~5m -2. Again, this is the lower limit of
the density. The real dislocation density during defor-
mation must be higher. It is difficult to provide
reliable statistics in such a complex structure, but Fig. 4. Typical microstructures of SMG copper after com-
there is evidence that the average dislocation pression to 29% (a), 53% (b) and 83% (c).
 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER
slips of less than 7 dislocations are not resolved. After
a deformation of 50% slip lines became better defined
and the operation of two slip systems was often
observed (Fig. 5). The average shear in the slip traces
were determined from the width of the shadow and
was estimated to be 6 nm after a deformation of 53%.
This corresponds to a contribution of 25% to the
total deformation.
An important feature of SMG copper after defor-
mation, as observed by replica techniques, is the
flattening of grains along the direction perpendicular
to the compression axis (Fig. 5), i.e. the grain shape
changes observed is consistent with the sample shape
change. This observation indicates that intragranular
slips make the main contribution to the total defor-
mation.
The study of replicas also revealed the formation of
steps in GBs due to GB sliding (GBs). As one can see
in Fig. 5(b), for instance, that GBS occurred not only
along one GB but also along several neighbouring
grains (co-operative sliding). The contribution of
GBS to total deformation was estimated by measur-
ing the step heights [18] to be in the range of 15-20%.
4. DISCUSSION
The experimental investigations have established
the following peculiarities in the plastic behaviour of
Fig. 5. Slip-line patterns and GB sliding traces on carbon
replicas from pre-polished surfaces of a sample which have
been deformed to 53%. The arrows indicate the direction of
platinum shadowing.
2471
SMG copper at room temperature: high yield and
flow stresses, very low strain hardening, low strain
rate sensitivity of the flow stress and high ductility.
These unusual mechanical properties, which are
not observed in coarse-grained materials, are
caused by specific processes taking place during the
deformation of SMG copper.
4.1. Deformation processes
Experimental results showed three processes oper-
ating during the deformation of SMG copper:
intragranular dislocation strain, grain boundary slid-
ing and GB migration, with the last process being
responsible for certain grain growth.
4.1.1. Dislocation strain. Dislocation slip inside
grains is clearly revealed by TEM observations of slip
traces on the surfaces of samples. Moreover, the
changes of grain shapes unambiguously show that the
intragranular strain makes the main contribution to
the total deformation of a sample. However, there is
no accumulation of dislocations in grains, although
their density is fairly high (approx. 1015m-2). There
may be two explanations for this.
First, a small amount of dislocations inside each
individual grain contributed to the deformation.
The number of dislocations which pass through a
grain in a unit time can be estimated with an
assumption that they are quickly trapped by GBs.
At a strain rate of 1.4 x 10-3s -1, as used in the
experiments, macroscopic deformation of 50% re-
quires a time interval about 360 s. Regarding the
grain size of 210 nm, this gives a grain elongation
of 105 nm, which corresponds to the slip of approx.
400 dislocations, i.e. one dislocation per second.
Second, the absence of dislocation accumulation
may be related to a recovery process. A part of this
recovery may be achieved by dislocation cross-slip.
Furthermore, the recovery must also take place as
a process of dislocation absorption in GBs. This
process is discussed in detail below.
The change of dislocation density, p, during the
deformation of fine-grain metals can be described by
the equation [26-28].
dp ~ p
- (1)
dt bd z
where b is the Burgers vector, d is the grain size, ~ is
the strain rate, z is the time required for dislocation
absorption by GBs and ~ is a geometrical term in
which the contribution of active dislocations and
the geometrical effect of dislocations are taken into
account [29].
The stationary solution of equation (1) is
P - bd (2)
therefore
pbd
= --. (3)
2472 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER
Substituting into equation (3) the following values
for the variables: p ~10[Sm -2, b = 2 . 5 x 10-1m,
d = 2 . 1 x 10-Tm, g = 1.4 x 10-3s -! and a = 2 . 4 in
accordance with [28] gives z = 15 s.
In recent years, a series of studies on GB absorp-
tion of dislocations have been carried out [28, 30, 31].
The models proposed in the cited works have ob-
tained expressions for the time of dislocation absorp-
tion. For instance, in [31] the following formula has
been obtained which complies with experimental data
0.03 k TH 3
= (4)
G llDb 6
where k, T, G have their usual meanings, 6 ,~ 10 -9 m
is the GB thickness, fl is the atomic volume and
H ~ 30 nm is the distance at which the image of a
dislocation disappears, D b is the GB diffusion co-
efficient. It is believed that the value of D b is consider-
ably different in U F G materials from that of
conventional materials. Its value is estimated using
equation (4) with the value of z determined by
equation (3). For T = 2 9 3 K , f~= 1.3 x 10-29m 3,
G = 48 GPa, it is obtained that Db = 3.5 x 10 -19 m2/s.
Assuming Db = Dbo exp(--Qb/RT), where, according
to [32], D b o = 2 . 3 5 x 10-SmE/s, a value Q b ~
78 kJ/mol is obtained for the GB diffusion activation
energy in U F G copper. In fact, the real value of Qb
may be slightly higher, since stationary dislocation
density is higher, as has been mentioned above.
For the density p ~ 2 x 10~Sm-2, for instance,
Qb ~ 79.2 kJ/mol would be obtained.
This value for GB diffusion activation energy is low
compared to the value of 107 kJ/mol for diffusion
along stationary GBs in coarse grained copper [32].
This implies that in the present situation the absorp-
tion of dislocations into GBs takes place in highly
non-equilibrium GBs in which the conditions for
diffusion are remarkably enhanced. Other defor-
mation processes related to GBs are analysed below.
4.1.2. Grain boundary migration and grain growth.
Grain growth was only observed during the process
of deformation in this study. To the contrast, no
grain growth was observed after a prolonged holding
time at room temperature. Such a grain growth
process is also observed during superplastic defor-
mation in conventional materials [33-35]. But, in the
case of low-temperature deformation of U F G metals,
this seems to have been observed for the first time.
Nevertheless, this is not a unique fact, since, for
instance, considerable grain growth has been ob-
served in pure nanocrystalline copper at room tem-
perature [36]. However, the nature of this grain
growth is not clear.
The kinetics of the grain growth in the U F G
copper is similar by character to that in conventional
materials. It is, apparently, related to the stimulated
GB migration. It is well known [35] that during
normal grain growth the change of average grain size,
d, obeys the law of
d = M F p with p ~> 1 (5)
where M = D b/kT describes the mobility of atoms in
GBs and F = (f~/6)(2v/d) is the driving force for the
process with ~, denoting the energy of GBs (the
surface tension of boundaries). During deformation,
there is an additional driving force related to the
elastic energy variation due to the annihilation
of extrinsic grain boundary dislocations and the
decrease of internal stresses
F = ~ - d~--~ (6)
where o9 oc PmBD/d is the elastic energy density of
extrinsic dislocations in the GBs. Assuming that the
density of extrinsic dislocations in remaining GBs
does not change during grain growth, the following
relation is obtained: d Oog/c~d= -o9. Since
og=a~/2E, where E is the Young's modulus,
equation (6) can be rewritten in the following form
r n{Zy tri2 )
= -~ ~,--~-+ ~ . (7)
Integrating equation (5) for p = 1 with F given by
equation (7), the following law for normal grain
growth is obtained
- = + (8)
where t is the time of deformation and do is the initial
grain size.
For a grain size in the range of 200-300 nm and
7 = 0.625 Jm -2 [16], the value of the first term in
parentheses in equation (8), which represents the
contribution of surface energy, lies in between 4.2
and 6.3 MPa. Since internal stresses are always lower
than the applied stress, the maximum value of the
second term, which describes the effect of elastic
energy, can be estimated using the applied stress,
aappu~ = 500 MPa; thus for E = 130 GPa, it gives that
tr2/2E = 1 MPa, which is less than 20% of the value
of 27/d. Therefore, the elastic term in equation (8) can
be neglected as compared to the GB surface energy.
Based on this consideration, grain growth curves for
two situations have been calculated using equation
(8) and plotted in Fig. 3. Curve 1 is for usual values
of diffusion parameters, Dbo = 2.35 x 10 -5 m2/s and
Qb = 107kJmol-k As can be seen from this curve,
grain growth does not occur in this case. Curve 2 is
for an activation energy Qb = 70 kJmol- i. This theor-
etical prediction is in agreement with the experimen-
tal results of the present study and the data reported
in [37], where it is shown that grain growth in
nanocrystals at low temperatures is associated with a
lower activation energy rather than high driving
forces.
4.1.3. Grain boundary sliding. High resolution
replicas were used for the observation of GBS, which
are usually difficult to be observed under conven-
tional conditions due to the very small grain sizes of
 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER
U F G materials. Although the contribution of GBS to
total deformation is not large (15-20%), GBS is an
important deformation process in U F G copper.
It is believed that GBS is controlled by GB diffu-
sion, although the micromechanism of GBS is not yet
fully understood, as expressed in the following
equation [34, 38]
~ Db "~( tr ) 2 ( b ) 2 . (9)
~Bs'~ A \ k T J \ E
This equation is valid when GBS is accommodated
and controlled by the plasticity of neighbouring
grains and the mechanism of the accommodation
is controlled by GB diffusion. Substituting
tr = 500 MPa, E = 130GPa and A = 1.5 x 103 [39]
into equation (9), an agreement with experimental
data is achieved for Qb = 73 kJmol -~.
Thus, for all the three deformation processes re-
lated to GBs, i.e. absorption of lattice dislocations,
GB migration and GB sliding, the estimated values
correspond well to experimental results when an
enhanced diffusion coefficient is adopted. The esti-
mations carried out in this study are simple and
appear reliable, although they may be a little surpris-
ing. Indeed, the decrease of GB diffusion activation
energy up to 70-78 kJ/mol is significant. Neverthe-
less, one can attempt to explain it by the recent results
on GB studies in U F G materials and taking into
account the deformation conditions of U F G copper
and the large internal stresses.
TEM, H R E M and dilatometric studies on GBs for
a number of U F G metals and alloys prepared by
severe plastic deformation [9, 1 !, 40] seem to have
proved the existence of highly non-equilibrium GBs
with high energy, excess volume and long-range stress
fields. This can be accounted for in terms of disor-
dered extrinsic GB dislocation arrays of extremely
high density [41]. With high internal pressure, it is
expected that diffusion is considerably accelerated in
GB regions. This unique feature of GBs in the
material under investigation is revealed by TEM
observations: most of the GBs having very high
dislocation densities or a specific diffraction contrast.
Recent studies have reported results on a remarkable
decrease in elastic moduli of the same material [16]
and a nuclear magnetic resonance measurement of
an activation enthalpy of 67 kJ/mol for a nano-
crystalline copper (grain size 10 nm) [42]. Both these
two observations can be rationalized in terms of
non-equilibrium GB conditions.
4.2. Mechanical behaviour
As has been pointed out above, a few unusual
features in the mechanical behaviour of U F G copper
have been observed, such as a high yield stress, a
narrow strain hardening region followed by a long
stage stable flow at a very low strain hardening rate,
high flow stress and high ductility.
4.2. I. Yield and flow stress. In this study very high
values of yield and flow stresses have been recorded
2473
for the U F G copper. In contrast, a considerably
lower value of yield stress was measured in a
nanocrystalline copper material [12]. The relatively
low yield stress in the nanocrystalline copper material
was probably due to the porosity of the nanocrys-
talline structure and thus did not reflect its inherent
property [10]. On the other hand, a flow stress of
about 350MPa was obtained in copper with
large area reduction (more than 80%) by extrusion
[43].
As has been estimated above, that approximately
one dislocation passes through each grain per second,
the high value of yield stress observed cannot be
explained by the dislocation pile-up approach. For
this reason, a recent model on the mechanical be-
haviour of nanocrystalline materials based on the
dislocation bow-out mechanism seems to be most
suitable [44]. According to this model, the critical
condition for yield to process is when dislocation
loops attain their semicircle configuration. The criti-
cal stress required for this condition is expressed
as [45]
-l+ 5 (10)
where M is the Taylor factor, v is the Poisson ratio
and L is the average dislocation length, which de-
pends either on the grain size when grains are in
nanometer scale or on the total dislocation density p
for grains larger then 100nm, through a simple
relation L = I/x/p [46].
For b = 2.56 x 10 -l m, G = 48 GPa, v = 0.35 and
M = 3.06, stresses of 357 and 427 MPa can be calcu-
lated using equation (10) for p = 5 10 t4 and
1015m 2, respectively. These values are smaller than
the measured yield stress of 390 MPa and flow stress
of 500MPa, by about 10-15%. This may be ex-
plained in terms of internal stresses which are not
considered in the equation, as well as that the real
dislocation densities are higher than the measured
ones.
According to this model, the strain hardening in
the initial stage of deformation (up to 5%) can be
interpreted as due to an increase in dislocation den-
sity from 5 x 10 t4 to 1015 m 2. The increase of internal
stresses influences the generation of dislocations im-
peding their bow-out and thus increasing the applied
stress necessary to continue the deformation. At the
same time, the increase in internal hydrostatic
pressure in tension activates GB diffusion and, as
a consequence, facilitates the recovery processes.
This results in the transition to a steady state of
deformation.
4.2.2. Steady state deformation. This stage is gov-
erned by the balance between the processes of strain
hardening and recovery in GBs. The recovery is a
process including the absorption of dislocations by
GBs, GBS and GB migration. The flow stress in
this stage is controlled by the dislocation bow-out
mechanism.
2474 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER
The results of this study may also provide reference
information on the nature of work hardening ob-
served at very large strains in stage IV for other
materials. Some similarities can be found between the
deformation behaviour of U F G copper and those of
conventional materials in stage IV, such as high flow
stresses, absence of strain hardening and low strain
rate sensitivities [14]. Furthermore, the formation of
fine-grain structures is also observed [14, 15]. The
mechanical behaviour in this stage has been exten-
sively studied for m a n y metallic materials, but little
attention has been paid to the effect of the structure
and properties of GBs. However, in the present case,
non-equilibrium grain boundaries as observed are not
a substructure as at the beginning of stage IV.
Furthermore, the high internal stresses may affect
the grain boundary diffusion energy: pb 3 equal to
0.17 eV with internal pressure in tension p equal to
1000 MPa.
5. CONCLUSIONS
1. Peculiar features in the mechanical behaviour
have been observed during the room-tempera-
ture compression for U F G copper with a grain
size of 210 nm. These features include high yield
stress, long steady state flow with very low
strain hardening and comparatively high duct-
ility.
2. The operation of multi-mechanisms, including
intragranular dislocation slip, grain boundary
sliding and migration, is responsible to the
unique deformation behaviour of the U F G
copper material in the steady state flow stage.
GB migration is capable of inducing certain
grain growth. In the steady state deformation
the density of the dislocations remains nearly
constant at a level as high as 1015m -2.
3. The recovery process caused by non-equilibrium
GBs, i.e. GB sliding and migration, can only
take place under conditions of enhanced GB
diffusion, due to high internal hydrostatic press-
ure in tension.
4. The high yield and flow stresses observed in the
submicrocrystalline copper interpreted by the
dislocation bow-out model, considering the
observation of the absence of significant
dislocation pile-up.
Acknowledgements--The authors would like to express their
thanks to the Chinese Education Commission and the
Institut National Polytechnique de Grenoble for financing
Professor J. Lian's participation in this work, to the Min-
istry of Researches and Space of France for its financial
sponsorship to Dr A. A. Nazarov, and to Dr Y. Liu for
fruitful discussions.
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