Metal Science and Heat Treatment Vol. 50, Nos.

7 8, 2008

STRAIN AND FRACTURE

UDC 621.7.01:669.3

INHERITANCE OF IMPERFECTIONS AND CYCLING OF STRUCTURAL

REARRANGEMENTS IN COPPER DURING DYNAMIC
RECRYSTALLIZATION UNDER CONDITIONS OF HOT PRESSING1

B. K. Barakhtin,2 N. R. Vargasov,3 and N. V. Lebedeva2

Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 8, pp. 34 38, August, 2008.

Structural changes in polycrystalline copper in the process of uniaxial compression at a rate of 10 3 102 sec 1
at 900C are studied with the aim to determine the conditions under which the mechanism of dynamic
recrystallization is a dominant one. Results of processing of images obtained by the methods of light and elec-
tron transmission microscopy and of data of quantitative metallography with 2D and 3D reconstructions are
used to suggest a scenario of cyclic changes in the structure, which promote the appearance of sources of dy-
namic recrystallization. Latent energy is assumed to be the driving force of the structural rearrangements.

INTRODUCTION ber of unstrained small-size grains in the strained metal. This

It is known [1] that hot pressure treatment is accompa-
nied by simultaneous development of the processes dynamic
return and dynamic recrystallization in metallic materials. In
accordance with the theory of heat treatment of metals [2]
the term dynamic return characterizes the phenomena of
recovery of the structural state, which lead to steady plastic
yielding of the metal at constant stresses. The term dynamic
recrystallization describes the processes characterized by an
inhomogeneous structure of grains and their boundaries and
the appearance of colonies of new grains. The special fea-
tures of crystallographic slip or, more accurately, the energy
of packing defects (EPD) determine the dominating process
and the kind of the formed grain structure. For example, in
metals with low EPD (Cu, Ni, g-Fe, etc.) the transverse slip
and the dislocation creep, which are the main mechanisms of
dynamic return, are hindered. For this reason the critical dis-
location density required for the beginning of dynamic
recrystallization is attained comparatively easily. This pro-
motes the appearance of colonies that consist of a great num-
1 conditions of steady plastic yielding of many metals and are
The paper is based on the report delivered at the Second Interna-
tional Conference Deformation and Fracture of Materials and
Nanomaterials (Moscow, 2007).
2 undergo polymorphic phase transformations during cooling,
St. Petersburg State Marine Engineering University (SPbGMTU),
St. Petersburg, Russia.
3
Sevmashvtuz Branch of SPbGMTU, Severodvinsk, Russia.
creates conditions for the phenomenon of superplasticity,
when the metal is capable to be strained by hundreds of per-
cent without loosing its continuity. The experiments con-
nected with processes of hot deformation are often aimed at
determining the conditions of manifestation of dynamic
recrystallization and using the possibilities of the super-
plastic state of the metal.
In the present work we determined the conditions of hot
plastic compressive deformation of polycrystalline copper
under which the mechanism of dynamic recrystallization is a
dominant one.
METHODS OF STUDY
We used cylindrical specimens with diameter D0 = 8 mm
and height h0 = 10 mm produced from technically pure cop-
per of grade M0. The specimens were deformed in a plastic
manner by uniaxial compression to a strain degree e = 0.4
[ez = ln (h/h0 )] in an Imash-56 device at a temperature of
900C at deformation rates ranging within &e = 10 3
102 sec 1. These parameters of hot deformation meet the
typical for industrial pressure treatment.
Copper was chosen as a test material because it does not
and therefore the structure fixed by quenching reflects the
actual state of the metal and is in fact a model one.

391
0026-0673/08/0708-0391 2008 Springer Science + Business Media, Inc.
392
100 mm 100 mm
a b
Fig. 1. Microstructure of copper in the center of specimens deformed at 900C at a rate of: a) e& = 10 1 sec 3; b ) e& = 10 1 sec 1;
c) e& = 102 sec 1.
N N b tribution of the grain sizes (see Figs. 1 3). For example, in
t1 t1
t2 > t1 t2 > t1
t3 > t2 t3 > t2
Dm Dm
Fig. 2. Diagrams of the distribution functions due to secondary re-
crystallization (a) and recrystallization (b ) at various moments of
time ti : Dm ) mean grain size; N ) specific number of grains of the
given size.
In order to study the microstructure of the central vo-
lumes of a specimen, where the plastic form variation is the
closest to the condition of uniform yielding (flow), we fabri-
cated analytical samples with metallographic polished sec-
tions and foils. The structure was studied by the methods of
quantitative metallography using an Axiovert light micro-
scope and the Expert Pro software and a Jeol 200 trans-
mission electron microscope.4 In order to minimize the pos-
sible artifacts appearing in the stage of preparation of the
samples, the specimens after mechanical grinding and pol-
ishing in a Sapfir 350E device were subjected to electro-
lytic polishing in a Kristall 620 electrochemical cell and
then to chemical uncovering of the grain structure in an alco-
holic solution of ferric chloride.
RESULTS AND DISCUSSION
As could be expected, in the center of the specimens,
where the straining was the highest, the formed grain struc-
ture consisted of almost equiaxed grains with polymodal dis-
4 most strained volumes were occupied by large grains. We
The electron microscopic study has been performed by T. N. Ale-
kseeva.
B. K. Barakhtin et al.
100 mm
c
the very center of a polished section a large crystallized grain
about 500 mm in diameter surrounded by numerous fine
(about 20 mm) grains was observed among grains 125
150 mm in size that corresponded to the initial (undeformed)
state (Fig. 1). This fact reflected the occurrence of active pro-
cesses of secondary and dynamic recrystallization in the cen-
tral volumes of the specimens.
Processing quantitatively the images of the structures we
established that the positions of some maxima in the distribu-
tions of the grain sizes depended on the deformation rate. For
example, the maxima corresponding to large grains displaced
toward greater sizes from 250 50 mm at &e = 10 3 sec 1 to
420 50 mm at &e = 102 sec 1, which was a result of secon-
dary recrystallization. Near the maxima of the initial grains
(125 150 mm) we detected a satellite, i.e., a peak the posi-
tion of which corresponded to a range of 80 20 mm (Fig. 3).
The changes in the rate of the deformation did not change the
position of the satellite but its height changed.
We had not intended to study the structural changes that
occurred by the mechanism of secondary recrystallization.
Therefore, we considered only those parts of the size distri-
bution functions which characterized small grains with a size
ranging within 50 150 mm. The maxima M0 that corre-
sponded to the grains in the initial state and the near-lying
satellite peaks C were located in these very parts. An indirect
proof of correctness of the choice of this scale for subsequent
analysis was the redistribution of the heights M0 and C of
the peaks, i.e., a decrease in one of the peaks was accompa-
nied by growth in the other, which is typical for processes of
dynamic recrystallization.
The parameters of the distributions (the height and the
half-width of the peaks) showed that plastic deformation at
900C at a rate of &e = 102 sec 1 in the assigned range of hot
compression modes was the closest to the condition of
superplasticity; the fraction of fine grains in the corre-
sponding copper specimen was the greatest, i.e., N = 13%.
In almost all of the deformed specimens the central and
were interested in determining the places of formation of
Inheritance of Imperfections and Cycling of Structural Rearrangements in Copper 393

N, %
40 When investigating the electrolytically polished micro-
sections we established (see Fig. 4) that the images of their
35
macro- and meso-textures contained orderly located indivi-
30
dual etched clusters or chains composed of clusters, which in
25
their turn were oriented in the direction of plastic deforma-
20 tion. The mean size of the clusters was 9 2 mm, though the
15 diameter of some of them attained 30 mm.
10 Within the fields of view of the microscope the propor-
5 tion of the area S taken by the etched clusters varied depend-
0 ing on the deformation rate. For example, after deformation
450 400 350 300 250 200 150 100 50 0
with &e = 10 3, 10 1, and 102 sec 1 the proportion of the
N, %
35 b etched places S = 25, 22, and 30% respectively (the value of
S was determined accurate to 3%). These special features
30
showed that the defects observed were connected with the
25
mode of plastic deformation of the specimens. Adequacy of
20 this assumption was confirmed by steady positive correlation
15 between the proportions of the areas S of the clusters and the
10 heights P of the stellite peaks for the small-diameter grains
5 formed by the mechanism of dynamic recrystallization
0 (Fig. 5).
450 400 350 300 250 200 150 100 50 0 The correlation equation derived by the least squares
N, % method has the form
35 c
30 S = 0.9P + 18.
25
20 It can be seen from the equation that in the initial state,
15 where the processes of dynamic recrystallization are not acti-
10 vated (P = 0), the structure of the metal already contains po-
5 tential sources, i.e., nuclei of further dynamic recrystalli-
0
zation (S = 18%).
450 400 350 300 250 200 150 100 50 0 It should be noted that the specimens have been pro-
D, mm duced from technically pure copper that could bear impuri-
Fig. 3. Polymodal distributions of the sizes of grains in the structure ties capable to cause inherited erosion. However, in this
of copper. The arrow points in the direction of the displacement of case the statistically uniform distribution of the impurity
maxima as a result of secondary recrystallization: a) rate of defor- would have prevented the observed deformation rate sensi-
mation e& = 10 3 sec 1; b ) e& = 10 1 sec 1; c) e& = 102 sec 1. tivity of the area of the affected regions. In addition, the ori-
entation of the eroded areas in the direction of plastic defor-
mation and the presence of positive correlation with the
small-size dynamically recrystallized grains as potential height of the satellite peak are obvious indicators of a rela-
sources of generation of the effect of superplasticity. tion between the etched clusters and the processes of active

100 mm

0.5 mm

a b

Fig. 4. Macro- (a) and meso- (b ) scale figures on etched surfaces in the form of clusters and chains on electrolytically polished
sections after compression of the specimen at t = 900C and e& = 10 3 sec 1. The direction of the deformation is shown by the
arrow.
394
S, %
32
30
28
26
24
y = 0.8878x + 18.306
22
20
0 5 10 15
P, %
Fig. 5. Correlation relation between the proportion of the area S oc-
cupied by etched clusters and the height P of the peak on the size dis-
tribution of small grains in the structure of copper.
plastic straining. A like effect is described in [3], where the
shape of etched dimples is studied in deformation of NiAl
crystals.
We thus assumed that the primary physical cause of the
appearance of orderly oriented etched figures was the latent
energy as the driving force of local dissolution of the metal.
We presume that the value of the latent energy is determined
by the contribution of two terms. The first term characterizes
the energy connected with the impurities and imperfections
of the structure (S = 18%) left from the earlier stages of treat-
ment of the preform. This inherited part of the latent en-
ergy manifests itself in the form of oriented channels of plas-
tic strain. The second active term corresponds to the con-
tribution of the energy (about 0.9P ) caused by the appear-
ance of sources of dynamic recrystallization due to the gen-
eration, accumulation, and self-organization of crystal struc-
ture defects as a result of crystallographic and accommoda-
tive plastic microstrain.
Adequacy of this assumption is indirectly confirmed by
the results of the consideration of superimposed images of
cluster chains observed on electrolytically polished micro-
sections and in the structure of grains uncovered by chemical
etching (see Fig. 6). The trajectories of the oriented erosions
coincided only partially with the contours of grain bounda-
Fig. 6. Microstructure of copper obtained by superimposition of images of unetched and etched polished sections of a specimen
deformed at e& = 10 3 sec 1 at t = 900C: a) 100; b ) 400.
B. K. Barakhtin et al.
ries, which is typical for structures of dynamic recrystalli-
zation [4]. Large localized erosions were located near junc-
tions of grain boundaries.
The assumption in question was also confirmed by the
results of the electron microscope study of the structure of
the metal. They showed that the main processes in the evolu-
tion of the internal structure of the metal occurred inside the
grains at a mesoscale level. For example, in hot
(tdef = 900C) compressive deformation at a rate &e = 10 3
102 sec 1 the grains acquired a cellular dislocation structure
with subgrain boundaries of different morphology. Spe-
cifically, after deformation with &e = 10 3 sec 1 the cells
with a size exceeding 1 mm were nonequiaxed (1 : 2); the
width of their boundaries did not exceed 200 nm, and most
of the boundaries had a broken appearance (Fig. 7a ),
which is typical for processes of fragmentation occurring at
high plastic strain. Deformation with &e = 10 1 sec 1 caused
formation of equiaxed cells with a size of about 1 mm with
shaggy boundaries up to 500 nm wide. In some places the
boundaries of the cells were characterized by thick diffrac-
tion contrast repeated with a step of about 300 nm, which re-
flected cyclic ordering of the structure of the boundaries
(Fig. 7b ).
After deformation at a rate &e = 102 sec 1 we detected
large (about 1 mm) cells separated by wide (about 600 nm)
boundaries inside which we observed cells up to 10 nm in di-
ameter (Fig. 7c ).
When studying electropolished but unetched micro-
sections we established that in many cases the shape and the
structure of an individual cluster possessed spherical symme-
try. As a rule, the polishing electrolyte affected the central
part of a cluster less than its boundary. This fact shows that
the latent energy is higher in the boundary G of a cluster and
that the structure of its core is resistant to the action of the
ions of the solution. In a chemically homogeneous material
the matrix can be made passive due to local amorphization of
the structure, which is the most possible in the stress field of
a disclination due to its splitting. For this reason we may as-
sume that large clusters appear as a result of selective disso-
lution at the places of junction disclinations and that the fine
erosions arranged into chains appear due to splitting of
a b
Inheritance of Imperfections and Cycling of Structural Rearrangements in Copper 395

q0, i
1 mm

w
1 mm q0, i + w

1 mm

1 mm c

Fig. 7. Dislocation structures formed after compression of copper at 900C and their schematic representation: a) com-
pression rate e& = 10 3 sec 1; b ) e& = 10 1 sec 1; c) e& = 102 sec 1.

disclinations lying on grain boundaries or in strain channels fections on the places of activation of subsequent dynamic
(Fig. 8). processes.
If the structural changes in hot deformation are accompa-
nied by splitting of junction disclinations and local amor-
phization of the structure, the amorphous regions should
grow in the process of continuing plastic straining and again
acquire crystalline properties. Later on, when located in a
channel of plastic strain, these volumes can be fragmented
b
again by new dislocation-disclination ensembles, and the re-
arrangement process will repeat. Such a model of structural
rearrangements is illustrated by a three-dimensional (3D) re- G
construction of etched clusters and chains (Fig. 9).
The 3D images show that the structural changes detected
in etched chains, individual clusters, and their boundaries oc-
cur in a cyclic manner. Successive alternation of regions of
active etching and passivation of the metal are detectable in c d
the diameters and shapes of concentrically arranged circles
formed by chains of etched dimples. The model suggested Fig. 8. Possible variant of linear splitting of a disclination lying on a
grain boundary or in a strain channel (a); disclination in a ternary
does not contradict the known data on the nature of dynamic junction (b ); schematic representation of the presence of a contour-
recrystallization with participation of active dislocations [4]. ing boundary G (c) in a cluster and of splitting of a junction
The data obtained by the method of quantitative metallo- disclination into an ensemble of less powerful disclinations with an
graphy show the possibility of influence of inherited imper- amorphous region in the center (d ).
396 B. K. Barakhtin et al.

Z Z Z

Y X
X Y X
Y
b c

Y
X

d e

Fig. 9. Three-dimensional reconstruction of regions of images with clusters detected on polished microsections of
specimens after deformation at t = 900C and e& = 10 3 sec 1 (a), e& = 10 1 sec 1 (b ), and e& = 102 sec 1 (c) and
an individual cluster 50 mm in diameter (d ) with its 3D reconstruction (e).

CONCLUSIONS 3. In the places of occurrence of inherited imperfections

1. Compression of polycrystals of technical copper of
grade M0 at 900C is accompanied by processes of secondary
and dynamic recrystallization. In the deformation range of
&e = 10 3 102 sec 1 the contribution of dynamic recrystalli-
zation is the highest at &e = 102 sec 1.
2. We have detected features of inheritance of structural
imperfections that have appeared in earlier stages of treat-
ment of the semiproduct. In addition to crystal structure de-
fects, which are generated, accumulated, and self-organized
in the process of active plastic straining, the inherited imper-
fections also become centers of nucleation of new grains.
the formation of dynamically recrystallized grains occurs in
a cyclic manner.
REFERENCES
1. B. M. Drapkin, V. K. Kononenko, and V. F. Bezyazychnyi,
Properties of Alloys in Extreme State [in Russian], Mashino-
stroenie, Moscow (2004).
2. N. I. Novikov, The Theory of Heat Treatment of Metals [in Rus-
sian], Metallurgiya, Moscow (1978).
3. G. K. Baranova, Orientation etching of NiAl crystals, Zavod.
Lab., 67(7), 36 37 (2001).
4. M. A. Shtremel, The Strength of Alloys. Part 2. Straining
[in Russian], MISiS, Moscow (1997).