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Acta Materialia 56 (2008) 230–241

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Microstructural evolution and nanostructure formation

in copper during dynamic plastic deformation
at cryogenic temperatures
Y.S. Li, N.R. Tao *, K. Lu *

Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China

Received 1 May 2007; received in revised form 10 September 2007; accepted 12 September 2007
Available online 5 November 2007

Abstract

The microstructural evolution and formation mechanism of nanostructures in bulk pure Cu samples induced by dynamic plastic
deformation (DPD) at high strain rates and cryogenic temperatures were investigated using transmission electron microscopic charac-
terization. Three different mechanisms were identified for the plastic deformation and microstructural refinement, including dislocation
manipulation and rearrangement, deformation twinning forming nanoscale twin/matrix (T/M) lamellae in bundles, and shear banding in
the T/M lamellae. An increasing tendency of deformation twinning and shear banding was observed at higher strains. For strain e = 2.1,
a mixed nanostructure is formed in the DPD Cu bulk sample with nanoscale T/M lamellae making up about 33% of the volume and
nano-sized grains making up about 67%. The nanograins can be classified into three types in terms of their origin: (i) nanograins derived
from fragmentation of nanoscale T/M lamellae with an average transverse size of about 47 nm; (ii) nanograins in shear bands with an
average transverse size of about 75 nm; and (iii) nanograins derived from dislocation cells with an average transverse size of about
121 nm. The high density of deformation twins induced by high strain rates and cryogenic temperatures in DPD, distinct from that
in conventional severe plastic deformation, plays a crucial role in formation of the nano-sized grains.
 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Nanostructured materials; Copper; Dynamic plastic deformation; Deformation twinning; Shear banding

1. Introduction are other processes known to produce true nanostructured

Owing to the growing interest in nanostructured materi-
als in recent years, numerous synthesis techniques have
been proposed [1]. Severe plastic deformation (SPD) pro-
cesses (e.g. equal channel angular pressing (ECAP) and
high-pressure torsion (HPT) [2–4]) are arguably the most
promising methods for producing bulk ultrafine-grained
metals while avoiding the consolidation step that often
brings artifacts into the samples [5]. However, the grain
sizes achieved so far through these routes for pure metals
such as Cu are usually outside the true nanoregime,
i.e. are of the order of several hundred nanometers. There
*
Corresponding authors. Tel.: +86 24 2390 6826; fax: +86 24 2399 8660.
E-mail addresses: nrtao@imr.ac.cn (N.R. Tao), lu@imr.ac.cn (K. Lu).
pure metals based on plastic straining, such as ball milling
(BM) [6], friction deformation under large sliding loads [7],
surface mechanical attrition treatment (SMAT) [8] and
cryogenic rolling [9]. However, these processes are either
inadequate for producing bulk samples and/or time-
consuming and costly. In short, difficulties in fabricating
bulk nanostructured samples expediently are a major road-
block for research and development of nanostructured
metals and alloys [10].
Recently, we have developed a new technique, dynamic
plastic deformation (DPD), i.e. plastic deformation at high
strain rates [11]. After the DPD process, high-density
nanoscale deformation twins together with nano-sized
grains are introduced into copper. The nanostructured
copper has a yield strength of 600 MPa, while keeping

1359-6454/$30.00  2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.actamat.2007.09.020
 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241
some plasticity. It is imperative to understand the micro-
structure evolution and formation of nanostructures in
copper during a DPD process from a scientific and techno-
logical point of view.
Strain-induced microstructural evolution has been exten-
sively investigated in numerous materials [6–10,12]. It has
been well documented that for those materials with medium
to high stacking fault energies (SFEs), such as Fe, Cu and
Al, coarse grains are refined upon continued straining by
various dislocation activities at low strain rates and at ambi-
ent temperatures. On the other hand, deformation twinning
is found to be an effective grain refinement mode in many
low SFE face-centered cubic (fcc) materials [13–15]. Never-
theless, when pure Cu with a medium SFE is deformed at
cryogenic temperatures and/or at high strain rates, defor-
mation twinning may play an important role in accommo-
dating plastic strain as dislocation activity is suppressed
[16–19]. However, little work has been done to study the
microstructural evolution in copper during high-strain-rate
deformation at cryogenic temperatures before.
The formation process of nanostructures in copper has
been investigated several times [9,20,21]. Nanocrystalline
structures can be introduced into copper by cold rolling
to very large extensions at cryogenic temperatures, and for-
mation of nanostructures is attributed to dynamic recrys-
tallization [9]. Extremely fine grains (<100 nm) can be
achieved in copper by means of either BM [20] or by
SMAT [21]. Formation of deformation twins and shear
bands is responsible for the structure refinement in the
BM process, and the high density of nanoscale twins is
believed to play a crucial role in the grain refinement in
the SMAT process.
The objective of the present work was to study the
microstructure evolution and nanostructure development
in pure Cu subjected to DPD at cryogenic temperatures,
which is of significance for both the fundamental under-
standing and technological applications of the DPD
processes.
2. Experimental
2.1. Sample
Copper cylinders (9 mm in diameter and 12 mm in thick-
ness) with a purity of 99.995 wt.% were used as raw mate-
rial for DPD treatment. Prior to the DPD treatment, the
Cu cylinders were annealed in vacuum at 973 K for 2 h
to diminish the effect of mechanical processing and obtain
homogeneous coarse grains. The grain sizes of the as-
annealed sample were within the range of 100–250 lm
and annealing twins were found in some grains (Fig. 1a).
2.2. DPD treatment
The DPD treatment was performed on a dynamic com-
pression facility. A copper cylinder sample placed on a
lower anvil was compressed by an upper impact anvil at
231
a high loading rate. The load and loading rate are con-
trolled automatically by a computer. Multiple impacts were
applied to deform a cylinder sample eventually to a disc of
about 1.5 mm thick. The strain rate applied in each impact
is estimated to be within 1 · 102–2 · 103 s1. The treated
sample was cooled by liquid nitrogen before each impact
and the sample temperature was estimated to be below
100 C during each impact.
The deformation strain is defined as e = ln (L0/Lf),
where L0 and Lf are the initial and final thickness of the
deformed sample, respectively. Measurements showed that
the Cu samples after DPD treatments are identical in den-
sity and purity to the original sample. No flaws (cracks or
porosities) have been detected inside the DPD samples. The
microstructure is rather uniform in the DPD samples both
in radius direction and along the thickness.
2.3. Microstructure characterization
An optical microscope (OM, Leica MPS 30) was used to
observe the holistic microstructure of the deformed Cu
specimens. For OM observations, the samples were etched
in a solution containing HNO3, H3PO4 and H4C2O5 (with
a ratio of 1:1:1) for 5 s. The detailed microstructures and
quantitative microstructure statistics of the samples were
characterized by means of transmission electron micros-
copy (TEM) and high-resolution transmission electron
microscopy (HRTEM), performed on a JEOL 2010 high-
resolution transmission electron microscope at an operat-
ing voltage of 200 kV. The cross-sectional thin foils for
TEM observations were prepared by means of double-jet
electrolytic polishing in an electrolyte consisting of 25%
(volume) alcohol, 25% phosphorus acid and 50% deionized
water at about 10 C.
3. Results and discussion
Fig. 1b–d shows cross-sectional optical micrographs of
the DPD samples with different levels of strain. Appar-
ently, the equiaxed coarse grains in the original as-annealed
sample were pancaked into flat grains perpendicular to the
loading direction. With an increasing strain, grains become
more flat and refined. Statistical measurements of the lon-
gitudinal (DL, perpendicular to loading direction) and
transverse grain sizes (DT, parallel to loading direction)
indicated that the average DL/DT ratio increases with
strain, from 1 (original) to about 3.5 for e = 1.1, as shown
in Fig. 1e. The plastic deformation, as evidenced by the dif-
ference in contrast, seems to be inhomogeneous in different
grains and even in different regions of the same grain.
Detailed microscopic characterization of the deformed
structures is given below.
3.1. DPD Cu sample with e = 0.4
The optical micrograph image of the DPD sample with
e = 0.4 is composed of two distinct types of regions with
232 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241

a ε= 0 b ε = 0.4 12 e
G 8
ε = 0.4

Loading direction
4
W
0

Frequency (%)
12

200 μm 200 μm 8 ε = 0.7

4
c ε = 1.1 d ε = 2.1
0

Loading direction
Loading direction

12

8 ε = 1.1
D 4

0
200 μm 200 μm 1 2 3 4 5 6 7
D /D
L T

Fig. 1. (a–d) Cross-sectional metallographic observations of the DPD Cu samples with different strains: (a) e = 0 (as-annealed), (b) e = 0.4, (c) e = 1.1 and
(d) e = 2.1. The letters ‘‘W’’ ‘‘G’’ and ‘‘D’’ denote the white region (hard-to-etch), the gray region (easy-to-etch) and the dark-gray region (very-easy-to-
etch), respectively. (e) Distribution of aspect ratios of grain sizes (DL/DT) in the three samples with different strains.

different contrasts: ‘‘white’’ (i.e. hard-to-etch) regions sim-
ilar to that in the original sample (e.g. a region labeled with
‘‘W’’ in Fig. 1b) and ‘‘gray’’ (easy-to-etch) regions (labeled
as ‘‘G’’ in Fig. 1b). The total area fraction of the ‘‘white’’
regions is apparently larger than that of the ‘‘gray’’ regions
in this sample. The gray regions are not distributed homo-
geneously throughout the whole sample.
Close observation showed that no obvious structural
feature is seen in the W region (Fig. 2a). In the G region,
some parallel bands are detected in a deformed grain
(Fig. 2b). These bands seem to initiate from the grain
boundary (GB) on the left-hand side and terminate inside
the grain (as indicated by black arrows) or at the GB on
the other side of the grain (indicated by white arrows).
Occasionally, terminations at annealing twinning bound-
aries are also visible in some grains. These band structures
indicate inhomogeneous deformation inside the grains.
Cross-sectional TEM observations of this sample
revealed that a high density of dislocations cells (DCs)
exists in most grains (Fig. 3a). The DCs do not seem to
be well developed and their sizes are of several hundred
nanometers. The cell walls are rather chaotic regions with
a high density of dislocations, while the cell interior has rel-
atively fewer dislocations. The corresponding selected area
electron diffraction (SAED) pattern, similar to that of a
copper single crystal, indicates that the misorientation
across the DC walls is negligible. This morphology is anal-
ogous to that observed in conventionally deformed Cu that
resulted from cross-slips of dislocations [22].
In addition to DCs, numerous deformation twins were
found in the form of bundles embedded in some deformed
grains, as evidenced in Fig. 3b. An SAED pattern along a
[0 1 1] zone axis from the twin bundles (Fig. 3c) showed the
superposition of a couple of Æ0 1 1æ diffraction patterns
which are symmetrical to each other with respect to the
{1 1 1} plane, indicative of a typical twin relationship
({1 1 1}/[1 1 2] type) among the lamellae. These twin/matrix
(T/M) lamellae form bundles with a total width of several
hundreds of nanometers and a length of several microme-
ters to several tens of micrometers. The measured statistic

Fig. 2. High-magnification metallographic images of the W region (a) and the G region (b) as indicated in Fig. 1b (e = 0.4).
 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241
a b
c 15
022T
200M
000
Fig. 3. (a, b) Typical cross-sectional bright field TEM images for the DPD Cu sample with e = 0.4. The corresponding SAED pattern for (a) is shown in
the inset. The SAED pattern and its index of the twin bundles in (b) are shown in (c). (d) The measured statistic distribution of the T/M lamellar thickness.
thickness distribution for the T/M lamellae from TEM
observations (Fig. 3d) is characterized by a normal loga-
rithmic distribution within a range from several to
150 nm. The mean thickness is approximately 47 nm. It fol-
lows from many of the TEM images that the volume frac-
tion of twinning region is about 10% in the deformed
sample (e = 0.4).
From the observed microstructure characteristics, we
identified that the hard-to-etch (white) regions under opti-
cal microscopy observations correspond to deformed
grains with DCs and the easy-to-etch (gray) regions to
the deformed grains with deformation twins. Actually the
observed bands in Fig. 2b are from deformation twin
bundles.
Dislocation slip and deformation twinning are two typi-
cal plastic deformation modes for fcc Cu. Dislocation activ-
ities are thermally activated processes. Various dislocation
configurations, including dislocation cells, walls, geometri-
cally necessary boundaries (GNBs) and incidental disloca-
tion boundaries (IDBs), are formed via manipulation and
rearrangement of dislocations when a polycrystalline Cu
is deformed at room temperature or above (e.g. in cold roll-
ing [22] or ECAP [23]). However, when deformed at lower
temperatures, dislocation manipulation and rearrangement
are suppressed, leading to formation of some poorly devel-
oped dislocation cells and a small number of microbands.
Another consequence of suppressed dislocation activi-
ties is that deformation twinning becomes more significant
in carrying plastic strain during DPD at cryogenic temper-
atures. The local stress required to nucleate deformation
twinning in Cu is high. In order to reach such a high local
233
400 nm 400 nm
20
d
Volume fraction (%)
222M,T
111M,T
022M
200T
10
0
0 40 80 120 160
T/M lamellar thickness (nm)
stress, sufficient strain hardening (or dislocation density) is
needed [24,25]. The present TEM result (Fig. 3b) confirmed
that appreciably plastic deformation by slip takes place
prior to activating deformation twinning. It is also seen
that severe deformation primarily occurs near GBs or
annealing twinning boundaries (TBs), where deformation
twins are preferred to form when the critical stress for twin-
ning is exceeded. With an increasing strain, the critical
stress of twinning can be achieved in more and more
strain-hardened grains. The population of deformation
twins thereby increases, as presented later.
Formation of nanoscale deformation twins in the DPD
Cu samples is distinct from that in the SPD Cu samples
deformed at low strain rates and ambient temperatures,
in which few deformation twins are formed. Structure evo-
lution and refinement in SPD Cu samples are carried out
primarily via dislocation activities with negligible twinning
deformation. Obviously, the high strain rate and cryogenic
deformation temperatures in the DPD process are key
parameters for forming a high density of nanoscale defor-
mation twins, both of which are essential for suppressing
dislocation activities. The large plastic strain is another fac-
tor to enhance the twinning processes because of a substan-
tial strain-hardening of grains. As will be demonstrated in
the following sections, more deformation twins are formed
in subsequent straining.
3.2. DPD Cu sample with e = 1.1
With increasing deformation strain, the gray regions
expand at an expense of the white, indicating that more
234 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241

T/M lamella bundles are formed. In the sample with

e = 1.1, some ‘‘dark gray’’ regions (labeled as ‘‘D’’ in a
Fig. 1c) appeared in addition to the white and gray regions,
as seen in Fig. 1b. The area fraction of white regions is con-

Loading direction
siderably decreased.
The presence of ‘‘dark gray’’ regions means that the
local structure is very easy to etch. A close look at the
‘‘dark gray’’ regions revealed that high density parallel
bands (analogous to that seen in gray regions, i.e. T/M
lamellae) exist, as seen in Fig. 4a. Within the parallel T/
M lamellae a few distinct bands are visible which intersect
the T/M lamellae with an angle of about 20–30. These
bands are separated by a spacing of about a few microme-
ters to a few tens of micrometers. Some bands ‘‘cut’’ 20 μm
through the whole twinned region, and some terminated
within the twin bundle. The morphology implies that shear
banding might have occurred within the twin bundles. This b
has been verified by cross-sectional TEM observations, as
shown in Fig. 4b, in which a shear band about 300 nm wide
is present in the nano-sized T/M bundle. Within the shear
band, nano-sized grains are detected. The T/M lamellae
become clearly curved in the vicinity of the shear band.
The thickness and orientation of the shear bands vary SB
considerably from grain to grain and even in a single grain.
The intersection angles between the shear bands and T/M
lamellae determined from metallographic observations
over a large volume of the sample, within a range of
15–35 (as shown in Fig. 4c), are consistent with those 400 nm
determined from TEM observations. TEM measurements
showed that the thickness of shear bands varies from 30
100 nm to several micrometers. The lengths of shear bands
are mostly dependent on the width of the twin bundles they
c
25
shear. Since the twin bundles are usually constricted within
one grain, the shear bands should be intragranular. 20
Frequency (%)

Detailed analysis of characteristics of shear bands are pre-

sented in Section 3.3.2.
15
Shear banding is a kind of instability which often
emerges when homogeneous plastic deformation cannot
10
sustain work hardening. This deformation mode frequently
appears in hard materials such as nanocrystalline materials
[26] and amorphous alloys [27]. In the nanoscale T/M 5

lamella bundles, where further work hardening becomes

very difficult, localized deformation in the form of shear 0
10 15 20 25 30 35 40
banding appears at stress concentrations within the bundle.
θ (degree)
Sharp boundaries are seen between the shear band and the
unsheared (T/M) region. In the vicinity of the shear band Fig. 4. (a) A magnified metallographic image of the D region outlined in
boundaries, T/M lamellae become curved to fit the shear- Fig. 1(c), showing several shear bands in the highly twinned region. (b) A
ing direction. typical TEM image showing a shear band that intersects with the T/M
The characteristics of shear bands are determined by lamellae. (c) Measured statistic distribution (from optical microscopy and
TEM observations) for the intersection angles between shear bands and T/
many factors, including the deformation temperature,
M lamellae.
strain rate, and the crystallographic structure etc. [28].
Due to the ample slip systems, dislocation slip is usually
the main deformation carrier in copper. Shear bands are [29]. In the present DPD process, dislocation activities are
found uncommonly ‘‘cutting’’ the microband matrix in severely suppressed, as discussed above. Moreover, the T/
heavily rolled copper. This type of shear band is usually M lamellae are so fine that it is difficult to activate disloca-
formed in metals with a high or medium SFE and is based tions or to refine the T/M lamellae by forming additional
on dislocation matrix; it is called a copper-type shear band microtwins. Consequently, further straining of the
 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241 235

nanoscale T/M lamellae is accommodated by shear band-
ing. This type of shear band is often formed in materials
with a medium to low SFE and is based on twinning
matrix; it is called a ‘‘brass-type’’ shear band [29].
Formation of an S-band, a band of intense local crystal-
lographic glide, was found in rolled Ni and Al [30]. During
traditional plastic deformation, S-bands usually appear
earlier than shear bands and are more dense than them.
During the DPD at cryogenic temperatures, dislocation
glide is suppressed, making it difficult for the traditional
S-band to form. The deformation was predominantly from
twinning and shear banding in DPD Cu at medium to high
strains.
It is generally believed that a decrease in deformation
temperature of fcc metals has a effect similar to decreasing
SFE, which is verified by the present result. That is, during
deformation at high strain rates and at cryogenic tempera-
tures, the microstructure evolution in copper is similar to
that of low SFE fcc metals, following a sequence of dislo-
cation–twinning–shear banding [31].
3.3. DPD Cu sample with e = 2.1
For the sample with e = 2.1, the deformation structure is
rather blurred but more homogeneous when compared
with that of copper deformed to small or medium strain
(Fig. 1a–c), and microstructure identification becomes very
difficult under OM, as seen in Fig. 1d. To clarify the e = 2.1
sample’s microstructure, cross-sectional TEM observations
were performed.
Fig. 5a and b are representative TEM micrographs from
this sample. It is obvious that the microstructure is com-
posed of nanometer-thick T/M lamellae and nanometer-
sized grains (crystallites). The nanoscale T/M lamellae,
which are perpendicular to the deformation direction, are
in the form of bundles in which several shear bands are

Fig. 5. (a, b) Typical cross-sectional bright field TEM images for the DPD Cu sample with e = 2.1. The microstructure consists of nano-sized T/M
lamellae and three types of nano-sized crystallites as indicated and described in the text.
236 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241

formed (as indicated in Fig. 5a). The density of shear bands

in this sample is much higher than that in e = 1.1. Statistic a
TEM measurements showed that the volume fraction of T/
M lamellae is about 33%, with nano-sized grains constitut-
ing the remaining volume.
TEM characterization of the T/M lamellae (Fig. 6a and
b) indicated that there are high-density dislocations locat-
ing at the TBs, typical of deformation twins. This is dis-
tinct from the growth twin structure in the same material
in which no dislocation exists at TBs [32]. The TBs are
highly stressed due to presence of numerous dislocations,
as evidenced by the HRTEM images (Fig. 6b). SAED pat-
terns indicate the same twin relationship as obtained in the
sample with e = 0.4. The T/M lamellar thickness is identi- 50 nm
cal to that in the sample with e = 0.4, as shown by the sta-
tistical measurements from TEM observations (Fig. 6c),
with an average value of about 49 nm. This means that, b
with an increase in the plastic strain, no thickening process
of the deformation twins occurs in the subsequent DPD
process. In other words, the T/M lamellae thickness is
insensitive to the degree of strain under the present DPD
conditions.
Nano-sized grains are found in three different types of
regions, indicating their different formation paths. The for-
mation mechanisms for these three types of nano-sized
grains are analyzed in following sections.

3.3.1. Nano-sized grains type (I): fragmentation of T/M

lamellae 4 nm
Within the T/M lamella bundles, discontinuous and
elongated ‘‘bamboo-like’’ nano-sized crystallites are identi- 20
fied, distinct from the continuous T/M lamellae structure, c
as shown in Figs. 5a and 7. From the dark field TEM image
and electron diffraction one can see that the nano-sized 15
grains possess random orientations (Fig. 7b and c). The
Volume fraction (%)

statistical measurement of the grain sizes of the nanograins,

as shown in Fig. 7e, indicated that the average transverse
grain size is about 47 nm and the longitude size is a few
hundred nanometers, with an average value of 119 nm
(the average aspect ratio is about 2.5). It is worth noting
that the average transverse grain size is coincident with
the T/M lamellar thickness (49 nm).
Micro-area electron diffraction within a very small vol-
ume (small circle in Fig. 7a) indicated that between the
adjacent grains, the fcc twin orientation relationships still
exist. These results indicate clearly that the discontinuous
grains are evolved from continuous T/M lamellae which
were subdivided during subsequent deformation. Plenty
of TEM observations showed that the total volume frac-
tion of this type of nano-sized grains is roughly about
30% in the whole sample.
Formation of nano-sized grains in nanothick T/M
lamellae, i.e. fragmentation of T/M lamellae, resulted from
dislocation–TB interactions. When plastic strain is applied
to the T/M lamellae, dislocation walls/tangles are devel-
oped within the lamellae, which subdivide the 2D T/M lay-
ers into discontinuous blocks, the orientations of which are
10
5
0
0 40 80 120 160
T/M lamellar thickness (nm)
Fig. 6. (a) A close TEM observation of the T/M lamellae in the DPD Cu
with e = 2.1. (b) An HRTEM image from the region outlined in (a).
(c) Statistic distribution of the T/M lamellar thickness in the sample
determined from TEM observations.
also changed due to accumulation of increasing number of
dislocations at boundaries. These blocks will gradually
evolve into randomly orientated grains. Such a grain refine-
ment process involving the interactions of twins and dislo-
cations has been evidenced in an Ni-based alloy [14] and
pure copper [21] subjected to the SMAT processing.
 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241 237

a b

400 nm

32
25
c e

Frequency (%)
24
20
16

15 8

0
10 0 4 8
Volume fraction (%) dL/dT

5 Transverse (dT)

0
25

d 20

15
Longitudinal (dL)
10

0
0 100 200 300 400 500
Grain size (nm)

Fig. 7. TEM observations of nano-sized crystallites derived from T/M lamellae in the DPD Cu sample with e = 2.1. (a) A bright-field image; (b) a dark-
field image; (c) an SAED pattern corresponding to the large circle in (a); (d) an SAED pattern corresponding to the small circle in (a). (e) Statistical grain
size (both transverse and longitudinal) distribution for the type-I nano-sized grains. The distribution of aspect ratio for the nanograins is shown in the inset
of (e).

Nano-sized grains can be obtained in the top surface of
SMAT Cu via fragmentations of deformation twins, which
shows that dislocation activities can operate within fine
twins with thickness as small as 10 nm [21].
The aspect ratio of most grains is larger than 2.0, mean-
ing that most grains are not equiaxed. If further straining is
applied to this sample, formation of more nanograins with
a smaller aspect ratio is anticipated. This has been verified
by our ongoing research [33].
3.3.2. Nano-sized grains type (II): inside shear bands
Nano-sized grains were found with each shear band, as
shown in Figs. 5a and 8. Most grains are elongated along
the shear direction and some are equiaxed. The transverse
grain size ranges from 20 to 200 nm, with an average of
75 nm. The longitudinal grain size is about twice that of
the transverse size (Fig. 8). In most cases, random orienta-
tions have been detected among the nanograins. The mea-
sured volume fraction of the nano-sized grains within shear
bands constitutes about 15%.
Systematic TEM observations showed that sizes and ori-
entations of the nanograins within shear bands vary with
the band width. Fig. 9a1–3 shows TEM micrographs of
three typical shear bands with widths (w) of 0.5, 1.2 and
3.8 lm, respectively. The microstructures inside each shear
band are characterized by nano-sized grains. From the cor-
responding SAED patterns inside the three shear bands, as
shown in Fig. 9b1–3, one may see different scenes. For the
thin shear band (a1) both random orientations and a typi-
cal fcc twin relationship can be detected. This means that
some of the grains still remain in the twinning connection
while others are randomly orientated within the thin shear
bands. For the thick bands, such as in a2 and a3, twinning
orientation is not obtainable and only random orientations
are seen, i.e. the original twin relationship in T/M lamellae
has been destroyed in these thick shear bands.
During shear banding, the original T/M lamellae might
be swept into the localized shearing region (band) at high
strain rates. The large degree of shear strain may induce
fragmentation and rotation of the T/M lamellae, forming
238 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241
a 10
200 nm
Fig. 8. (a) A typical bright field TEM image showing nano-sized crystallites in a shear band in the DPD Cu sample with e = 2.1. The inset shows the
corresponding SAED pattern. (b) measured statistic distribution of grain sizes (transverse and longitudinal) for the nano-sized grains inside shear bands.
The distribution of aspect ratio for the nanograins is shown in the inset of (b).
elongated (or equiaxed) crystallites. This may explain our
observation that twinning connections remained partially
between some adjacent crystallites. For the crystallites that
have undergone large degrees of rotation, the twin relations
are destroyed. However, one may not exclude the possibil-
ity of secondary twinning within shear bands of which the
strain rate is very high. This possibility has been noticed in
other alloy systems before [34].
Another observation is that grains in thin shear bands
are obviously smaller than those in thick bands. As shown
in Fig. 9c1–3 and d1–3, the average transverse grain size
increases from 57 nm (w < 0.5 lm) to about 74 nm
(0.5 < w < 1.5 lm) and 79 nm (w > 1.5 lm). A similar trend
is found for the longitudinal grain size. This observation
means that grain coarsening occurs simultaneously with
the thickening of shear bands.
Usually, severe plastic deformation at high strain rates
takes place within the adiabatic shear bands (narrow
regions of highly localized deformation which experience
unusually high levels of strain and strain rate) during their
formation and thickening processes in which a substantial
transient temperature rise may also be induced. The R c temper-
b
ature increase within a shear band is DT ¼ qc c0
s dc, in
which b = 0.9 (assuming 90% of work of deformation was
converted to heat), q is the density of the sample, c is the spe-
cific heat capacity and c0 is the shear strain for shear band
initiation. From the equation, the temperature increment
DT is related solely to that of the shear strain in a shear
band. The estimated transient temperature within shear
bands in Cu during plastic deformation at ambient temper-
ature is about 500 K [35]. Such a high thermal pulse might
induce grain coarsening or dynamic relaxation (or recrystal-
lization) in pure Cu [35]. Therefore, coarsening of nano-
grains might be activated mechanically by the large plastic
straining at high rates and/or thermally by the transient
temperature rises. Grain coarsening in shear bands is
14
b 25
Frequency (%)
12 20
15
10
8 5
6 0
Volume fraction (%)
0 2 4 6
dL/dT
4
2 Transverse (dT)
0
14
12
10 Longitudinal (dL)
8
6
4
2
0
0 100 200 300 400 500
Grain size (nm)
accompanied by softening. Thus, in subsequent straining,
deformation in existing shear bands may occur preferably
in the form of further shearing. This may lead to band thick-
ening and further grain coarsening following more mechan-
ical and thermal activations. Eventually, the grain sizes tend
to a saturated value, analogous to that in the SPD samples.
With an increasing number of shear bands, the T/M
lamella bundles formed earlier are progressively eroded.
Therefore, the volume fraction of T/M lamellae does not
increase monotonically with increasing strain. Instead, it
tends to saturate with further increasing strain (see Fig. 11a).
Shear bands intersecting pre-existing growth-in twins
have been reported in cold-rolling electrodeposited copper
[36]. The deformed structure inside the shear bands is
dominated by a lamellar dislocation structure typical for
cold-rolled samples. In shock-loaded Cu samples, ultrafine
grain formation in adiabatic shear bands has also been
observed [37]. Ultrafine grains are thought to be formed
via a dynamic recovery process, which helps formation
of elongated subgrains with low angle boundaries at early
stages of shear banding, followed by breakdown and split-
ting of the elongated crystallites into equiaxed crystallites
in the latter stage. Different from that in the shocked sam-
ples, shear bands in the DPD Cu sample are formed in
nanoscale T/M lamellae. Hence, formation of nanograins
in shear bands in the present DPD Cu may result primar-
ily from the breakdown of nanoscale T/M lamellae and
rotations of the fragmented crystallites. This seems to be
consistent with our observation that the grain sizes in
shear bands are very close to the T/M lamellar thickness,
which is much smaller than that in SPD samples (often
200 nm).
3.3.3. Nano-sized grains type (III): outside T/M lamellae
In addition to type-I and type-II nanograins, some
grains with sizes ranging from several tens of nanometers
 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241 239

a1 a2
DT
DT

SB SB
DT DT

500 nm 500 nm

DT
a3

SB

DT

500 nm

b1 b2 b3

24 c1 16 d1
18 12
w < 0.5 μm w < 0.5 μm
12 8

6 4

0 0
Volume fraction (%)
Volume fraction (%)

24 c2 16
d2
18 0.5 μm < w < 1.5 μm 12 0.5 μm < w < 1.5 μm
12 8

6 4

0 0
24 c3 16 d3
18 w > 1.5 μm 12 w > 1.5 μm
12 8

6 4

0 0
0 40 80 120 160 200 0 100 200 300 400
Grain size (perpendicular to SB, nm) Grain size (parallel to SB, nm)

Fig. 9. (a1–3) Typical TEM images of three shear bands with different widths (w) in the DPD Cu sample with e = 2.1. (b1–3) The corresponding SAED
patterns for the three shear bands. (c1–3, d1–3) Statistical distributions for the transverse and longitudinal sizes of the nano-sized grains inside shear bands
with different widths (c1 and d1: w < 0.5 lm, c2 and d2: 0.5 lm < w < 1.5 lm, c3 and d3: w > 1.5 lm), respectively, determined from a large number of
TEM images.
240 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241

a b
15

Volume fraction (%)

10

400 nm 0
0 50 100 150 200 250 300
Grain size (transverse, nm)

Fig. 10. (a) A typical TEM image showing the nano-sized grains outside T/M lamellae in the DPD Cu sample with e = 2.1. Inset is the corresponding
SAED pattern. (b) Measured statistic distribution of transverse sizes for the type-III nano-sized grains.

to submicrometers are observed outside the T/M lamella
bundles. Most of these grains are elongated with curved
boundaries and some are equiaxed, as shown in Fig. 10a.
Misorientations across the boundaries vary from a few
degrees to a few tens of degrees. High-density dislocations
are always observed in association with these grains. These
grains are obviously larger than type-I and type-II nano-
grains. The average transverse size of these grains is about
121 nm, as depicted in Fig. 10b. The longitude sizes range
from several submicrometers to micrometers. The total vol-
ume fraction of type-III grains is about 22%.
From the morphology and boundary misorientations,
one may find that the refined grains are evolved from
DCs, which is analogous to those in SPD Cu and in deep
layers of SMAT Cu samples [21] in which dislocation activ-
ities dominate the deformation and grain refinement pro-
cess. The sizes of this type of grain are comparable to
those obtained in SPD Cu [38]. Formation of these submi-
45 Twin volume fraction (%)
Twin volume (%)
cron-sized grains via dislocation manipulation and rear-
rangement implies that deformation twinning in these
regions has not been initiated, probably due to unfavorable
orientations of the original coarse grains or insufficient
local stress under the DPD conditions.
Fig. 11b depicts the variation of several characteristic
sizes in the DPD Cu samples with different strains. We
found that the T/M lamellar spacing does not change with
the plastic strain under the present experimental condi-
tions. The average sizes of three types of nanograins do
not seem to depend on the strain either.
Table 1 summarized the structure characteristics of the
DPD Cu sample with e = 2.1. Obviously this sample is
composed of a mixed nanostructure: about 33 vol.% nano-
scale twins (or T/M lamellae) with three types of nano-
sized grains. The average size of all grains is about
68 nm, which is much smaller than that in SPD Cu samples
[23,38].
Tensile test results showed that the DPD Cu sample
exhibits a high tensile yield strength of about 600 MPa
and an ultimate tensile strength of 633 MPa [11]. Both
a are much higher than those of SPD Cu samples (415

30
and 455 MPa, respectively [23]). In addition, the tensile
elongation-to-failure of the DPD Cu is about 11%,
15 which is comparable to that of the SPD Cu [23]. These
results indicate the DPD Cu sample may possess an
0 enhanced fracture toughness in comparison with the
T/M lamellar thickness
Transverse size of nano-grain I
b SPD Cu samples. Detailed investigations on the
120
Transverse size of nano-grain II mechanical behaviors of the DPD Cu samples are in
Transverse size of nano-grain III
progress [33,39].
Average size (nm)

90

60
Table 1
Volume fraction and average thickness (kT/M) for the T/M lamellae and
30 average sizes (dT: transverse size, dL: longitudinal size) for three types of
nanograins in the DPD Cu sample with e = 2.1, determined from cross-
0 sectional TEM observations
0.0 0.5 1.0 1.5 2.0
T/M lamellae Nano-sized grains
Strain
Type I Type II Type III
Fig. 11. Variation of volume fraction of T/M lamella bundles (a) and
Volume (%) 33 30 15 22
variation of several characteristic sizes (b) as a function of deformation
Average size (nm) kT/M = 49 dT = 47 dT = 75 dT = 121
strain, including average T/M lamellar thickness, transverse sizes for three
dL = 119 dL = 160
types of nanograins derived from different origins.
 Y.S. Li et al. / Acta Materialia 56 (2008) 230–241
4. Conclusions
Dynamic plastic deformation of bulk pure Cu samples
at cryogenic temperatures induces a significant microstruc-
tural evolution and formation of nanostructures. The dom-
inant mechanisms governing the plastic deformation and
microstructural refinement include dislocation manipula-
tion and rearrangement, deformation twinning forming
nanoscale T/M lamella bundles, and shear banding in the
T/M lamellae. At low strains, dislocation activities and
twinning dominate the deformation process. With increas-
ing plastic strain an obviously increasing tendency of defor-
mation twinning and shear banding was observed.
For strain e = 2.1, a mixed nanostructure is formed in
the DPD Cu sample with about 33 vol.% of nanoscale T/
M lamellae and 67 vol.% of nano-sized grains. The nano-
grains can be classified into three types in terms of their ori-
gin: (i) nanograins derived from fragmentation of
nanoscale T/M lamellae with an average transverse size
of about 47 nm; (ii) nanograins in shear bands with an
average transverse size of about 75 nm; and (iii) nanograins
derived from dislocation cells with an average transverse
size of about 121 nm. Obviously, deformation twinning
induced by high strain rates and cryogenic temperatures
in the DPD process plays a critical role in the microstruc-
tural evolution and formation of nanograins, which is the
fundamental difference from that in the conventional
SPD processes.
Acknowledgements
Financial supports from the National Natural Science
Foundation of China (Grant Nos. 50671106, 50621091
and 50431010) and the Ministry of Science and Technology
of China (Grant No. 2005CB623604) are acknowledged.
The authors thank Q.H. Lu, B. Wu, C.S. Hong and Y.
Zhang for stimulating discussions.
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