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2467-2475, 1994
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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.
2467
2468 VALIEV et al.: D E F O R M A T I O N BEHAVIOUR OF U F G COPPER
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 angle ones, as evident from a selected area electron
the samples is the presence of extinction contours diffraction pattern shown in Fig. 2(b). The pattern
inside many grains, indicating high internal stresses was taken from an area of 0.5/~m 2 and contains
[23]. Extinction contours are often observed in dislo- numerous spots arranged in circles like those from
cation-free grains. This suggests that the sources of typical polycrystals [24]. Moreover, recent TEM
the high internal stresses are in grain boundaries. examinations of SMG samples using micro-diffrac-
Such internal stresses have been observed by TEM tion analysis with the electron beam focused individ-
and X-ray techniques in a number of U F G materials ually on each grain provided evidences for high-angle
produced by severe plastic deformation [2, 9, 11]. misorientations between neighbouring grains [25].
The grain structures of the specimens are of gran- Recently, the formation of such a granular structure
ular type, i.e. the grain boundaries are mainly high- in Ni3AI after severe plastic deformation followed by
AM 42i7--S
2470 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER
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.
slips of less than 7 dislocations are not resolved. After SMG copper at room temperature: high yield and
a deformation of 50% slip lines became better defined flow stresses, very low strain hardening, low strain
and the operation of two slip systems was often rate sensitivity of the flow stress and high ductility.
observed (Fig. 5). The average shear in the slip traces These unusual mechanical properties, which are
were determined from the width of the shadow and not observed in coarse-grained materials, are
was estimated to be 6 nm after a deformation of 53%. caused by specific processes taking place during the
This corresponds to a contribution of 25% to the deformation of SMG copper.
total deformation.
4.1. Deformation processes
An important feature of SMG copper after defor-
mation, as observed by replica techniques, is the Experimental results showed three processes oper-
flattening of grains along the direction perpendicular ating during the deformation of SMG copper:
to the compression axis (Fig. 5), i.e. the grain shape intragranular dislocation strain, grain boundary slid-
changes observed is consistent with the sample shape ing and GB migration, with the last process being
change. This observation indicates that intragranular responsible for certain grain growth.
slips make the main contribution to the total defor- 4.1.1. Dislocation strain. Dislocation slip inside
mation. grains is clearly revealed by TEM observations of slip
The study of replicas also revealed the formation of traces on the surfaces of samples. Moreover, the
steps in GBs due to GB sliding (GBs). As one can see changes of grain shapes unambiguously show that the
in Fig. 5(b), for instance, that GBS occurred not only intragranular strain makes the main contribution to
along one GB but also along several neighbouring the total deformation of a sample. However, there is
grains (co-operative sliding). The contribution of no accumulation of dislocations in grains, although
GBS to total deformation was estimated by measur- their density is fairly high (approx. 1015m-2). There
ing the step heights [18] to be in the range of 15-20%. may be two explanations for this.
First, a small amount of dislocations inside each
4. DISCUSSION individual grain contributed to the deformation.
The number of dislocations which pass through a
The experimental investigations have established grain in a unit time can be estimated with an
the following peculiarities in the plastic behaviour of 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)
Substituting into equation (3) the following values d = M F p with p ~> 1 (5)
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 where M = D b/kT describes the mobility of atoms in
accordance with [28] gives z = 15 s. GBs and F = (f~/6)(2v/d) is the driving force for the
In recent years, a series of studies on GB absorp- process with ~, denoting the energy of GBs (the
tion of dislocations have been carried out [28, 30, 31]. surface tension of boundaries). During deformation,
The models proposed in the cited works have ob- there is an additional driving force related to the
tained expressions for the time of dislocation absorp- elastic energy variation due to the annihilation
tion. For instance, in [31] the following formula has of extrinsic grain boundary dislocations and the
been obtained which complies with experimental data decrease of internal stresses
U F G materials. Although the contribution of GBS to for the U F G copper. In contrast, a considerably
total deformation is not large (15-20%), GBS is an lower value of yield stress was measured in a
important deformation process in U F G copper. nanocrystalline copper material [12]. The relatively
It is believed that GBS is controlled by GB diffu- low yield stress in the nanocrystalline copper material
sion, although the micromechanism of GBS is not yet was probably due to the porosity of the nanocrys-
fully understood, as expressed in the following talline structure and thus did not reflect its inherent
equation [34, 38] property [10]. On the other hand, a flow stress of
about 350MPa was obtained in copper with
~ Db "~( tr ) 2 ( b ) 2 . (9)
~Bs'~ A \ k T J \ E large area reduction (more than 80%) by extrusion
[43].
This equation is valid when GBS is accommodated As has been estimated above, that approximately
and controlled by the plasticity of neighbouring one dislocation passes through each grain per second,
grains and the mechanism of the accommodation the high value of yield stress observed cannot be
is controlled by GB diffusion. Substituting explained by the dislocation pile-up approach. For
tr = 500 MPa, E = 130GPa and A = 1.5 x 103 [39] this reason, a recent model on the mechanical be-
into equation (9), an agreement with experimental haviour of nanocrystalline materials based on the
data is achieved for Qb = 73 kJmol -~. dislocation bow-out mechanism seems to be most
Thus, for all the three deformation processes re- suitable [44]. According to this model, the critical
lated to GBs, i.e. absorption of lattice dislocations, condition for yield to process is when dislocation
GB migration and GB sliding, the estimated values loops attain their semicircle configuration. The criti-
correspond well to experimental results when an cal stress required for this condition is expressed
enhanced diffusion coefficient is adopted. The esti- as [45]
mations carried out in this study are simple and
appear reliable, although they may be a little surpris- -l+ 5 (10)
ing. Indeed, the decrease of GB diffusion activation
energy up to 70-78 kJ/mol is significant. Neverthe- where M is the Taylor factor, v is the Poisson ratio
less, one can attempt to explain it by the recent results and L is the average dislocation length, which de-
on GB studies in U F G materials and taking into pends either on the grain size when grains are in
account the deformation conditions of U F G copper nanometer scale or on the total dislocation density p
and the large internal stresses. for grains larger then 100nm, through a simple
TEM, H R E M and dilatometric studies on GBs for relation L = I/x/p [46].
a number of U F G metals and alloys prepared by For b = 2.56 x 10 -l m, G = 48 GPa, v = 0.35 and
severe plastic deformation [9, 1 !, 40] seem to have M = 3.06, stresses of 357 and 427 MPa can be calcu-
proved the existence of highly non-equilibrium GBs lated using equation (10) for p = 5 10 t4 and
with high energy, excess volume and long-range stress 1015m 2, respectively. These values are smaller than
fields. This can be accounted for in terms of disor- the measured yield stress of 390 MPa and flow stress
dered extrinsic GB dislocation arrays of extremely of 500MPa, by about 10-15%. This may be ex-
high density [41]. With high internal pressure, it is plained in terms of internal stresses which are not
expected that diffusion is considerably accelerated in considered in the equation, as well as that the real
GB regions. This unique feature of GBs in the dislocation densities are higher than the measured
material under investigation is revealed by TEM ones.
observations: most of the GBs having very high According to this model, the strain hardening in
dislocation densities or a specific diffraction contrast. the initial stage of deformation (up to 5%) can be
Recent studies have reported results on a remarkable interpreted as due to an increase in dislocation den-
decrease in elastic moduli of the same material [16] sity from 5 x 10 t4 to 1015 m 2. The increase of internal
and a nuclear magnetic resonance measurement of stresses influences the generation of dislocations im-
an activation enthalpy of 67 kJ/mol for a nano- peding their bow-out and thus increasing the applied
crystalline copper (grain size 10 nm) [42]. Both these stress necessary to continue the deformation. At the
two observations can be rationalized in terms of same time, the increase in internal hydrostatic
non-equilibrium GB conditions. pressure in tension activates GB diffusion and, as
a consequence, facilitates the recovery processes.
4.2. Mechanical behaviour
This results in the transition to a steady state of
As has been pointed out above, a few unusual deformation.
features in the mechanical behaviour of U F G copper 4.2.2. Steady state deformation. This stage is gov-
have been observed, such as a high yield stress, a erned by the balance between the processes of strain
narrow strain hardening region followed by a long hardening and recovery in GBs. The recovery is a
stage stable flow at a very low strain hardening rate, process including the absorption of dislocations by
high flow stress and high ductility. GBs, GBS and GB migration. The flow stress in
4.2. I. Yield and flow stress. In this study very high this stage is controlled by the dislocation bow-out
values of yield and flow stresses have been recorded mechanism.
2474 VALIEV et al.: DEFORMATION BEHAVIOUR OF UFG COPPER
The results of this study may also provide reference 2. R. Z. Valiev, R. R. Mulyukov and A. V. Korznikov,
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