Materials Science and Engineering, A137 ( 1991 ) 35-40 35

Plastic deformation of alloys with submicron-grained structure

R. Z. Valiev, N. A. Krasiinikov and N. K. Tsenev
Institute for Metals Superplasticity Problems, U.S.S.R. Academy of Sciences, Khalturina 39, Ufa 450001 (U.S.S.R.)

Abstract

The peculiarities of a submicron-grained structure formation in a series of aluminium- and magnesium-

based alloys by means of a special strain-heat treatment are examined in this paper. The unusual
mechanical properties of alloys displayed in this state at room temperature as well as at enhanced tem-
peratures are found. The nature of the plastic deformation of these materials is discussed.

1. Introduction 2. Experimental details

Materials with superfine grains (nanocrystal-
line and submicron grains) possessing certain
unusual physicomechanical properties have lately
given rise to much interest among researchers
[1-5]. In particular, they are characterized by an
abnormally high diffusion activity [1, 2] and a
lower elasticity modulus [3], their superplastic
temperature sharply decreases [4], and in nano-
crystalline ceramics brittleness disappears at rela-
tively low temperatures [5]. Nanocrystalline
materials with a grain size of 0.01 pm or less are
usually produced by means of special powder
metallurgy techniques [1]. At the same time, to
produce submicron-grained (SMG) alloys with a
grain size of about 0.1 pm, high ultimate strains
can be used, with subsequent fixing of the initial
stages of recrystallization [2, 4, 6]. Such
strain-heat treatment has two main advantages: it
is applicable to a wide scope of metals and alloys,
commercial materials included, and no residual
porosity is found in the SMG samples produced.
In this connection, it would be interesting to study
the behaviour of the SMG alloys under deforma-
tion. Unfortunately, however, their mechanical
properties and nature of deformation are almost
unknown; it is not clear whether the Hall-Petch
relationship is applicable to them and no data on
the regularities of strain hardening are available.
It is also important to find out the dependence on
the temperature of deformation. This paper pre-
sents the first systematic investigations in these
matters undertaken on a number of aluminium
and magnesium alloys.
The aluminium alloys AI-4Cu-0.5Zr (model
alloy) and alloy 1420 (Al-5Mg-2Li-0.1Zr)
(commercial alloy) (where the compositions are
in approximate weight per cent) were used for the
investigations. Before deformation, the cast
ingots were subjected to homogenization anneal-
ing. The MA8 alloy (Mg-l.5Mn-0.3Ce) used
was a solid solution based on a-Mg with a small
amount of MggCe and fl-Mn particles (total,
2.5%) of size, about 0.05 pm and stable up to
800 K. To produce the SMG structure, the alloys
were subjected to high plastic strains at room
temperature by means of torsion straining under
a pressure of 6 GPa or to equal-channel-angular
pressing, the true logarithmic strains e being 4-7
[2, 4].
The transmission electron microscopy (TEM)
studies were conducted on a JEM-2000 EX
electron microscope. The density of dislocations
was measured at points where dislocations are at
the surface. The mechanical properties were
studied during the tensile straining of the samples
on a universal testing machine of Instron type, the
strain rate being constant.
3. Results
3.1. Formation of the submicron-grained alloy
structures
A detailed investigation of the SMG structure
formation was conducted on the A I - C u - Z r alloy
and MA8 alloy [7]. Figure l(a) shows a typical
aluminium alloy structure after high deformation.

0921-5093/91/$3.50 Elsevier Sequoia/Printed in The Netherlands

36
Fig. 1. Microstructures and diffraction patterns of
A I - C u - Z r alloy: (a) as-deformed, e = 7; (b) after addition
annealing at 493 K for 1 h.
It is evidently a well-formed grain (fragmented)
structure with a mean fragment size of about 0.2
/tm. This structure is characterized by the follow-
ing two features: first, there are almost no disloca-
tions within the fragments, but the extinction
contours are clearly seen, indicating large internal
stresses. Second, there is no banded contrast at
the fragment boundaries, characteristic of well-
formed grain boundaries observed by TEM. Evi-
dently, it is these fragment boundaries that
function as sources of internal stresses in the
alloy. From ref. 8, such non-equilibrium boun-
daries are known to be quite frequently observed
after plastic deformation and their origin is
related to the presence of grain boundary disloca-
tions and disclinations.
At the same time, according to experiments on
diffraction, the fragment boundaries have large-
angle misorientations. Figure l(a) presents an
electron diffraction pattern from a foil area of
about 0.5/~m 2. There are quite a number of ref-
lections arranged in circles. Such a diffraction
1
250
200
3
f
150
100
50
i i i i i i
0 0,02 0~04 0,06 OT08 0o10 0,12
Fig. 2. True stress-strain curves of magnesium alloy MA8,
Taler=293 K; g = 5 1 0 4 S I: curve 1, S M G structure,
d = 0.3 ktm, non-equilibrium grain boundaries; curve 2, S M G
structure, d = 0.3/~m, equilibrium grain boundaries; curve 3,
alloy with mean grain size d = 10/~m.
pattern provides direct evidence that consider-
able misorientations are present in the structure.
It may be claimed that the structure of an alloy
after high deformation consists of microfrag-
ments separated by large-angle boundaries.
These boundaries are largely non-equilibrium
and the density of defects is very high there.
The SMG structure looks slightly different
after additional annealing. By selecting special
modes of heating, a structure was produced with
almost the same grain size, but without any inter-
nal stresses and with a typical banded contrast at
the boundaries (Fig. l(b)). In this case, the
electron diffraction pattern also constains a large
number of reflections, but they have no azimuthal
spreading. These are evidently equilibrium grain
boundaries.
The patterns of the SMG structure formation
observed in the magnesium and AI-Li alloys
were quite similar.
3.2. Mechanical properties of submicron-grained
alloys at room temperature
Let us compare, for example, the deformation
behaviour of the MA8 alloys with submicron
(do = 0.3/~m) and fine (do = 10 ~m) grains. Figure
2 shows three typical stress-strain curves for the
alloy at 293 K. Curves 1 and 2 refer to SMG
structures distinguished by the states of grain
boundaries: non-equilibrium (curve 1) and rela-
tive equilibrium (curve 2) states. In this case, the
flow stresses are quite similar but there is a sharp
difference in the elongations to failure. Both the
 37

curves are devoid of pronounced strain harden- much higher than in a conventional state, the
ing and this is what distinguishes in principle the plasticity being sufficiently high (Table 1 ).
alloy behaviour from that of an alloy with a grain
size of 10/~m (curve 3). Also, in the latter case, 3.3. M e c h a n i c a l p r o p e r t i e s at elevated
the yield point value is much lower. temperatures; superplasticity
Figure 3 presents the 00.2 VS. d - 1/2 dependence Figure 5 presents the temperature depen-
characteristic of this alloy. For small grain sizes dences of the magnesium alloy yield stress when
the linear dependence of 00. 2 on d 1/2 is the grain sizes are 0.3 and 10 ,um. In the case
evidently preserved, but at grain sizes smaller when d~ = 10 ktm, a drop in the aq~2value occurs
than 0.5 /xm the slope of this dependence
changes. From these data the Hall-Petch rela- % 21,
tionship parameters can be evaluated: a0.2=
a o + k d -1/2. Assuming that a 0 is the same for
both segments, we obtain k ~= 0.075 MN m-1/2
and k H 0.025 MN m - 1/2.
=

To analyse the nature of the observed depen-

dence of 0o.2 on d-1/2, it would be interesting to
study the dislocation structure of samples
strained by 2% (Fig. 4). In the alloy structure with
a grain size of about 1/~m (Fig. 4(a)), dislocations
can be clearly seen both within the grains and in
the grain boundaries. Their average density is
(2-3)x 108 c m --2. At the same time, when the
grain size is 0.3/~m (Fig. 4(b)), the density of dis-
locations was less than 109 cm-2, the boundaries
containing no defects. Here, in many of the grain
boundaries, only a residual contrast left by dislo-
cations can be found (see A in Fig. 4(b)). As is
well known [8], such a contrast is associated with
the spreading and vanishing of the trapped lattice
dislocation images.
In the aluminium alloys, the highest flow stress
is observed with a grain size of 0.3 ,urn. Hence,
the creation of the SMG structure provides for
the realization of a rather high strength state in
them. Thus, for example, in the A1-Li commer-
cial alloy 1420 with a SMG structure, the yield
stress o0.2 and ultimate strength ost values are

iff'002 DI/~.
25o

200 j/

150

IO0

50

,oo ~o . I , oTs. or3' o..2. a,,~,,

0 0~4 ow8 112 lt6 210 2e4 J - 1 / 2 j j~ffl - 1 / 2
1
Fig. 4. Dislocation structure in magnesium alloy after 2%
Fig. 3. Yield stress as function of mean grain size in mag- tensile strain at room temperature: (a) d = 1 #m; (b) d = 0.3
nesium alloy M A 8 ( Tae e = 293 K). um.
38

at temperatures above 600-620 K (curve 2) and In the SMG aluminium alloys the superplastic
at 670 K the alloy displays superplastic features temperature is still lower. Thus, in the A I - C u - Z r
[8]. At the same time, when d0=0.3 ktm, an alloy, it decreases by almost 300 K (Table 2).
abrupt softening occurs in the temperature range Electron microscopy studies indicated that
350-400 K (crave 1) and the superplastic effect is structural changes occurring in the course of the
realized at 450 K (Table 2). The data presented deformation of SMG alloys are also typical of
indicate that the SMG alloy displays typical superplastic materials (Fig. 6). After deformation,
superplastic behaviour; its properties at 450 K grains remain equiaxial, no dislocations are found
are similar to the properties of this alloy with a in the structure, and certain growth of grains is
grain size of 10/~m displayed at 670 K. observed. Thus, after the 100% tensile straining,
the grain size was 0.5/~m.
TABLE 1 Hence, during the deformation of SMG alloys,
a typical superplastic behaviour can be observed.
Values of yield stress o 02 ultimate strength ast and maximum
elongation to failure in the submicron-grained alloys Since in this case the superplastic temperature
decreases by 200-250 K, we can speak of the so-
Alloy do o'0.2 ast 6 called relatively low temperature superplasticity
(/am) (MPa) (MPa) (%) of SMG materials.
AI-Cu-Zr 8 100 260 6
AI-Cu-Zr 0.3 220 300 9
4. Discussion
A l ~ l o y 1420 10 330 450 5
Alalloy1420 0.2 550 600 6 The data obtained indicate that intensive plas-
tic deformation provides for the formation of a
microfragmented structure in the alloys. Detailed
investigations of the structural changes under
6*" O) 2~IL?a high plastic deformations prove [7, 9] that micro-
fragments are formed owing to the development
200 of the rotational modes of deformation. The frag-
ment boundaries formed are rather non-equilib-
rium but, when heated, they are transformed into
large-angle grain boundaries. This is how the
100
SMG structure is assumed to be produced.
The SMG aluminium and magnesium alloys
under study display unconventional mechanical
behaviour, associated primarily with a reduction
. . . . . . . , , , , ,
in the Hall-Petch constant k, with the grain size
J, o 0 400 ~ 600 700 800 ~)K being less than 0.5 /~m. Quite recently, similar
features were discovered by Gleiter and co-
Fig. 5. Temperature dependence of the yield stress of mag-
nesium alloy MA8 ( g = 5 x 10 4 s-l): curve 1, d = 0 . 3 /~m; workers [10] while measuring the microhardness
curve 2, d = 10/~m. of nanocrystalline copper. These workers sup-

TABLE 2
Conditions and parameters of superplastic deformation of the alloys

Alloy d T g a20 m 6
(~um) (K) (s ') (MPa) (%)

AI-Cu-Zr 8 773 3 x 10 -4 13 0.50 800

AI-Cu-Zr 0.3 493 3 10 -4 23 0.48 > 250 a
AI-Cu-Zr 8 493 3 10 -4 37 0.19 80
Mg based (MA8) 10 673 5 x 10-4 25 0.42 320
Mg based (MA8) 0.3 453 5 10-4 33 0.38 > 150 a
Mg based (MA8) 10 453 5 x 10-4 100 0.25 80

aMeasurements were restricted by test conditions.


0.2 j~m
! !
Fig. 6. The structure of the SMG A I - C u - Z r alloy: (a) initial
state; (b) after superplastic deformation at e = 100%.
39
posed that the decrease in microhardness in the
region of very small grain sizes was due to the
development of Coble diffusion creep even at
room temperature. This point of view has not
been confirmed experimentally so far [i1].
Nevertheless, the data presented in this paper
give direct evidence for the increasing role of dif-
fusion processes at small grain sizes. Indeed, the
study of the 2% strained samples (see Fig. 4) has
indicated that, in the grain boundaries of the mag-
nesium alloy of 0.3/zm grain size, the spreading
of trapped lattice dislocations is observed, which
is not the case when the grain size is 1 /~m. It is
well known [8] that the spreading of dislocations
in the boundaries is the initial stage of their
absorption and is connected with diffusion. Thus
the increasing rate of dislocation spreading
implies the acceleration of grain boundary diffu-
sion in a SMG alloy. It should be noted that quite
recently this conclusion has been confirmed by
experimental measurements of diffusion param-
eters undertaken on SMG aluminium alloys [2].
From the point of view of enhanced diffusion
and accelerated absorption of lattice dislocations
by grain boundaries in the region of small grain
sizes, the basic peculiarities of mechanical pro-
perties observed are quite understandable. This
is, first of all, the absence of work hardening
which arises because, at room temperature,
deformation acquires the features of hot strain-
ing. Second, under the acceleration of grain boun-
dary diffusion, the conditions of strain transfer
across grain boundaries change, which results in a
change in the HalI-Petch constant.
The acceleration of diffusion in a SMG alloy is
also of important significance for the relatively
low temperature superplasticity to be displayed.
It is well known that superplasticity is related in
its nature to the combined development of the
following mechanisms of deformation: grain
boundary sliding and intragranular deformation
under enhanced diffusion. The dependence of
strain rate g on flow stress o can be described by
the following expression [8]:
~=kT
where A is a constant, o i is the threshold stresses,
D is the grain boundary diffusion coefficient and
all the other symbols have their usual meanings,
Using this equation and data included in Table
2, the ratio of the diffusion coefficient for "con-
40
ventional" to that for "low temperature" super-
plastic deformation in the aluminium alloy is
evaluated to be 103 .
At the same time, calculating the decrease in
the grain boundary diffusion coefficient which
occurs when the temperature drops from 773 to
493 K and taking into account the exponential
dependence of D on temperature, we obtain
D773/D493 = 5 X 104.
Thus during the deformation of SMG alloys
we observe a considerable acceleration of grain
boundary diffusion when the diffusion coefficient
is 1.5 orders of magnitude larger than that under
"conventional" deformation. Such an abnormal
growth of diffusion in SMG alloys is probably the
main factor determining the possibility of "low
temperature" superplasticity.
5. Conclusions
(1) The formation of the SMG structure
during intensive plastic deformation is associated
with the formation of microfragments, whose
boundaries are non-equilibrium and can be re-
structured into large-angle boundaries under sub-
sequent heating.
(2) The SMG alloys under study display
unusual mechanical behaviour: strain hardening
is not pronounced, and the Hall-Petch constant
decreases in the region of small grain sizes, owing
to the absorption of dislocations by grain bound-
aries because of accelerated diffusion in such
materials.
(3) The superplastic temperature drops con-
siderably in SMG alloys (by 200-300 K) owing to
the enhancement of diffusion processes.
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