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Grain boundary structure of
nanocrystalline Cu processed by
cryomilling
J. Y. Huang
a
, X. Z. Liao
a
, Y. T. Zhu
a
, F. Zhou
b
& E. J.
Lavernia
c
a
Materials Science and Technology Division , Los Alamos
National Laboratory , Los Alamos, New Mexico, 87545, USA
b
Department of Chemical and Biochemical Engineering
and Materials Science , University of California , Irvine,
California, 926971, USA
c
Department of Chemical Engineering and Materials Science ,
University of California , Davis, California, USA
Published online: 15 Nov 2010.
To cite this article: J. Y. Huang , X. Z. Liao , Y. T. Zhu , F. Zhou & E. J. Lavernia (2003) Grain
boundary structure of nanocrystalline Cu processed by cryomilling, Philosophical Magazine,
83:12, 1407-1419, DOI: 10.1080/1478643031000083633
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PHILOSOPHICAL MAGAZINE, 2003, VOL. 83, NO. 12, 14071419
Grain boundary structure of nanocrystalline Cu processed
by cryomilling
J. Y. Huangy, X. Z. Liao, Y. T. Zhu
Materials Science and Technology Division, Los Alamos National Laboratory
Los Alamos, New Mexico 87545, USA
F. Zhou
Department of Chemical and Biochemical Engineering and Materials Science,
University of California, Irvine, California 926971, USA
and E. J. Lavernia
Department of Chemical Engineering and Materials Science, University of
California, Davis, California, USA
[Received 18 January 2002 and accepted 31 December 2002]
Abstract
The microstructures of cryogenically ball-milled Cu were investigated by high-
resolution electron microscopy. It was found that the grain-size reduction is a
dislocation-controlled continuous process which consists of the formation of
small-angle grain boundaries (GBs), a gradual increase in misorientations as a
result of accumulation of more dislocations and, nally, the formation of large-
angle GBs. The GBs were generally curved, wavy or faceted, and heavily strained,
which are typical characteristics of nanostructured materials. In addition, extrinsic
dislocations were found in many GBs, indicating that most are in a high-energy
non-equilibrium conguration, which is consistent with observations in equal-
channel angular pressing processed Cu, Ni, and AlMg, repetitive corrugation
and straightening processed Cu and room-temperature ball-milled Cu. These
results support a still-disputed concept that GBs in nanostructured metals
processed by severe plastic deformation are mostly in non-equilibrium states.
} 1. Introduction
Ball milling has been proven to be a versatile technique for production of large
quantities of nanocrystalline powders which can be sucient for industrial applica-
tion. It is a typical top-down approach during which coarse-grained materials are
decomposed into nanocrystalline building blocks under severe plastic deformation.
Although this technique has been extensively used in both research laboratories and
industries to synthesize nanostructured materials, detailed microstructural evolution
during this process remains unclear, which severely hinders understanding and
further application of this technique. The grain sizes of the ball-milled powders are
usually less than 100 nm. Thus, conventional transmission electron microscopy inves-
Philosophical Magazine ISSN 14786435 print/ISSN 14786443 online # 2003 Taylor & Francis Ltd
http://www.tandf.co.uk/journals
DOI: 10.1080/1478643031000083633
{ Current address: Department of Physics, Boston College, Chestnut Hill, Massachusetts
02467, USA. Email: [email protected].
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tigation cannot provide much information regarding dislocation congurations or
grain boundary (GB) structures. In this context, high-resolution electron microscopy
(HREM), which can provide atomic-scale structural information, is stringent. So far
only limited eort has been given to the atomic structural investigation of ball-milled
materials (Huang et al: 1994a,b, 1996, 1997a,b, 1998a,b, Shen et al: 1995, Huang
1999, Yang et al: 1999, 2000). This is possibly because ball-milled powders are usually
agglomerated to large dense particles of micron scale, which makes it very dicult to
obtain a thin region of a few nanometres or a tenth of a nanometre that is suitable for
HREM. This makes it impractical to observe the ball-milled powders directly.
Nevertheless, two techniques have been developed to obtain high-quality HREM
samples (Huang et al: 1994a,b). These techniques have proved to be versatile ways
to obtain directly atomic-scale structural information of the milled powders. Another
practical way to obtain high-quality samples suitable for HREM is the following: the
milled powder was cold compacted to a pellet and then ion milling or jet polishing was
applied. This technique is suitable for ductile metals, such as Cu, Al and Zn.
Applying the above techniques, numerous deformation structures produced by
ball milling have been revealed. For example, we observed room-temperature
deformation twins in ball-milled Cu (Huang et al. 1996), which is unusual since
Cu has enough slip systems (12) to accommodate the deformation at room
temperature. We also observed nanograins deforming by simultaneous shearing
rather than by the normal dislocation slip under high strain rates induced by ball
milling (Huang et al: 1998a). These results provide not only deep insight into the
ball-milling process but also new understanding of nanostructured materials.
The GB structure of nanostructured metals processed by severe plastic deforma-
tion is suggested to be in a non-equilibrium state (Horita et al: 1996, 1998, Huang
et al: 2001, Valiev et al: 2000). The non-equilibrium GBs were proposed to be char-
acterized by the presence of high density of extrinsic defects, such as dislocations and
vacancies (Valiev et al: 2000). However, direct evidence of non-equilibrium GBs was
not present until recently (Huang et al: 2001). Huang et al: (2001) found that extrin-
sic dislocations that are not geometrically necessary indeed exist in the GBs of Cu
processed by repetitive corrugation and straightening (RCS). It is interesting to
investigate whether the GBs in ball-milled nanostructured materials are also in
non-equilibrium states. It is also practically important to investigate the GB
structure of dierent nanostructured materials, since the change of GB structure
can result in the change of physical and mechanical properties.
We report in this paper atomic-scale GB structure of nanostructured Cu after
cryogenic ball milling in liquid N
2
. The GB structure is compared with those
observed in other cold deformation techniques, such as equal-channel angular-
pressing (ECAP) (Horita et al: 1996, 1998) and RCS (Huang et al: 2001).
} 2. Experimental procedure
A commercial Cu powder (99.5%+pure) with a particle size of about 300 mesh
was used for the milling experiments. The milling was carried out in a modied
Union Process 01-HD attritor with a stainless steel vial and balls (6.4 mm in
diameter) at a rate of 180 rev min
1
for 8 h. The ball-to-powder weight ratio was
40 to 1. During the milling operation, liquid N
2
was added into the mill to maintain
complete immersion of the milling media, which keeps the temperature at 1968C.
The as-milled powders were cold compacted to a disc of diameter 4.4 mm under a
pressure of about 3 GPa. The disc was then mechanically polished to a thickness of
1408 J. Y. Huang et al.
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about 20 mm and then ion milled for about 1 h suitable for HREM observation. The
HREM experiment was carried out in a JEOL 2010F electron microscope operated at
200 kV. The grain sizes were normally less than 100 nm so that tilting of individual
grains was very dicult. Thus, HREM images were taken randomly in a number of
grains.
} 3. Results
3.1. Grain size and general morphology
The grain size of the cryomilled Cu was not homogenous, and it varied from
region to region. The morphology of the grains also changed dramatically in
GB structure of cryomilled nanocrystalline Cu 1409
Figure 1. (a)(e) A general morphology of cryomilled Cu with dierent grain sizes and
morphologies. (e) A representative electron diraction from the nanograins.
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dierent regions. Typical transmission electron micrographs are shown in gures
1 (a)(d). In gure 1 (a), the grain size is approximately 1020 nm, which is the smal-
lest grain size observed in this sample. The grain structures in gure 1 (b) are not well
developed, and the GBs are not well delineated, possibly owing to the extremely
irregular shape and overlapping of grains. The grain size in gure 1 (b) is about 70
80 nm, and this was the most frequently observed morphology in this sample. In
contrast with gure 1 (b), individual grains are well dened in gure 1 (c), and most
of the GBs are very sharp. The grain size in gure l (c) is larger than in gure 1 (b), and
the largest size is about 160 nm. Defects in the interior of grains are readily visible, as
indicated by the arrowheads. These defects are either stacking faults (SFs) or twins. In
a rare case, very large grains were observed, and a typical example is shown in gure
(d), which shows a grain of about 600 nm. The dislocation density in such a large grain
is very high, and cell structure is also visible. These results indicate that deformation
in the ball-milling process is not homogeneous. Figure l (e) is a representative electron
diraction pattern from the cryomilled Cu that shows diraction rings typical for
nanostructured materials. The diraction rings show 111 and 200 texture.
3.2. Defects in the grain interior
Dislocations were found in most large grains with sizes greater than 50 nm. The
dislocations identied by HREM were mostly of a 608 mobile type; these are typical
dislocations in Cu after deformation (Huang et al. 1996, 2001). Besides dislocations,
another important defect frequently observed in cryomilled Cu is deformation twins,
an example of which is shown in gure 2. These multiple twins contain a giant step as
indicated by the arrowheads in gure 2. The lattice in the step region is incoherent.
Such a giant step can be associated with very complicated dislocation congurations.
We were unable to identify these dislocations because the image was not clear
enough to identify the core of the dislocations, and the step was possibly in a
non-equilibrium state.
1410 J. Y. Huang et al.
Figure 2. Deformation twins in cryomilled Cu. The arrowheads indicate a giant step.
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When deformed at room temperature, slip rather than twinning is the preferred
mode of deformation for Cu, because Cu has an intermediate SF energy, and twin-
ning is dicult to occur at room temperature condition. However, as pointed out by
Huang et al. (1996), under certain circumstances, such as a small grain size, high
strain rate and low temperature, twinning can become the preferred mode of
deformation. Deformation twins were found in ball-milled Cu even under room-
temperature conditions. In the present case, the milling was performed at liquid-
N
2
temperature so that deformation twinning occurs more readily.
3.3. Grain boundary structure
Figure 3 shows an asymmetric-tilt small-angle grain boundary (SAGB) and four
dislocations that are almost periodically distributed. If one assumes that the electron
beam is parallel to B 1

110, the Burgers vector of the dislocations is determined to

GB structure of cryomilled nanocrystalline Cu 1411
Figure 3. An asymmetrical SAGB. The white inverted Ts indicate the cores of the GB
dislocations.
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be b
1
2
10

11, which makes them 608 dislocations. Based on the simplied Frank
formula, the spacing of the dislocations can be calculated to be d b=, where is
the misorientation angle between the two grains and is about 68 in the present case.
The calculated spacing between dislocations is 2.42 nm, which agrees very well with
the experimental value of 2.45 nm. The SAGB is therefore well described by the
simplied Frank formula. This SAGB does not contain extrinsic dislocations and
is in equilibrium state.
Figure 4 is another asymmetrical tilt SAGB, and the misorientation angle is
about 68. The Burgers vector of the dislocations in the SAGB is again b
1
2
10

11.
The interesting point in this SAGB is that there are two intersecting SFs on the two
sets of {111} planes crossing the SAGB. As such, the SFs are bent after crossing the
SAGB. This means that the SAGB cannot prevent the propagation of dislocations.
The SFs are apparently generated by dissociation of two 608 dislocations, the cores
of which are indicated by two inverted white-edged black Ts and b
1
and b
2
.
We show how a SAGB is formed by the introduction of dislocations in gure 5.
The GB is outlined by two types of strip (some of which are indicated by white
arrowheads), which extend on the two sets of {111} planes. These strips are actually
SFs or thin twins, which are associated with the dissociation of two 608 dislocations,
1412 J. Y. Huang et al.
Figure 4. An asymmetrical SAGB. The white inverted Ts indicate the core of the GB
dislocations. SF
1
and SF
2
are two intersecting SFs. The Burgers vectors b
1

1
2
10

11
and b
2

1
2
101:
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as indicated by Ts in gure 5 (b). These dislocations are slightly dissociated, thus
producing the SFs and thin twins. The misorientation between the two grains is
about 28 because of the introduction of these dislocations. A similar SAGB was
also observed in ball-milled Cu (Huang et al. 1996) and in ECAP-processed Al
Mg (Horita et al: 1996).
Figure 6 shows a SAGB with a misorientation angle of approximately 16.58
reaching the limiting angle for that of a SAGB. The GB is curved and cannot
be described by the simplied Frank formula. However, the Burgers vector of
the GB dislocations is still a lattice vector, which is not the case for a large-
angle grain boundary (LAGB). It is thus reasonable to classify such a GB as a
SAGB. It is noted that for such a SAGB, the lattice is severely distorted in the
GB region.
Figure 7 shows a SAGB with a misorientation of about 108. The lattice spacing is
approximately 1.8 A

which corresponds to that of Cu(200). The GB plane is curved.

In order to locate cores of the mismatch dislocations, the original image in gure
7 (a) was Fourier ltered and shown in gure 7 (b), from which it is clearly seen that
many mismatch dislocations were present in the GB region. According to the
misorientation angle, the periodicity of the mismatch dislocations should be 66
lattice spacings. This means that geometrically necessary dislocations should appear
in every 66 (200) lattice spacings. However, the actual observed dislocation
periodicity is about 13 (200) lattice spacings, as seen in gure 7 (b). So many extrinsic
dislocations which are not geometrically necessary were present in the GB. This
infers that such a SAGB is a non-equilibrium GB.
GB structure of cryomilled nanocrystalline Cu 1413
Figure 5. (a) An asymmetrical SAGB; the white arrowhead indicate SFs or twins in the two
sets of {111} planes. (b) A local magnication of the region outlined in white in (a); the
white Ts indicate the cores of the GB dislocations.
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Figure 8 shows GBs among three grains. The misorientation angles between
grains 1 and 2, grains 2 and 3, and grains 3 and 1 are about 58, 198 and 118
respectively. The GB between grains 1 and 2 is a SAGB produced by dislocations,
while that between grains 2 and 3 appears to result from direct shearing, as evidenced
by the narrow band present in the GB. The GB between grains 1 and 3 is curved and
strained in several regions, and Moire fringes due to overlapping of the two grains
can also be seen.
Figure 9 is a near-symmetrical tilt SAGB. The dislocations are not aligned in one
lattice plane yet, and dislocations with opposite Burgers vectors are shown close to
each a other. Therefore, this segment of GB has a high energy and is in a non-
equilibrium state.
Figure 10 is a near S 11 LAGB. The GB plane is at and slightly strained.
Figure 11 shows a LAGB which exhibits a stepwise arrangement of facets parallel to
(111) planes, and each facet consists of four to six layers of (111) planes. In gure 12
are shown a number of grains and GBs. In grains 1 and 2, deformation twins are
seen. The deformation twins in grain 2 are initiated from the GB and terminated in
the interior of the grain, meaning that the GB is heavily strained, thus becoming a
nucleation site for other defects. The GB between grains 1 and 2 is a SAGB. The GBs
are generally curved and strained and, in several regions, lattice disordering is
observed.
1414 J. Y. Huang et al.
Figure 6. An asymmetrical SAGB. The T and inverted Ts indicate the cores of the GB
dislocations. The misorientation between the two grains is 16.58.
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GB structure of cryomilled nanocrystalline Cu 1415
Figure 7. An asymmetrical SAGB. (a) The original image; the arrowheads denote the GB.
Filtered image from a segment of (a); the arrowheads indicate the cores of the
mismatch dislocations.
Figure 8. GBs among three grains.
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1416 J. Y. Huang et al.
Figure 9. A near-symmetrical SAGB. The T and inverted Ts indicate the cores of the GB
dislocations.
Figure 10. A near S 11 GB. The GB plane is straight and slightly strained.
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GB structure of cryomilled nanocrystalline Cu 1417
Figure 11. A GB containing facets on (111) planes and steps.
Figure 12. Nanograins and GBs in cryomilled Cu. The arrowheads indicate SFs or thin
twins. Note that SFs or thin twins initiated from the GB and terminated in the interior
of grain 2. The white circles outline disordered regions in the GBs. The white-edge
black lines in the upper right corner indicate a twin. The numbers 16 indicate grains.
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} 4. Discussion
4.1. Grain renement mechanism during ball milling
The process of grain renement during large strain deformation has been dis-
cussed by Hughes and Hansen (1997), Hughes et al: (1997) and Zhu and Lowe
(2000). With increasing strain, cell blocks separated by geometrically necessary
boundaries form within grains and cellular structures with incidental dislocation
boundaries form within grains. The misorientations of geometrically necessary
boundaries and incidental dislocation boundaries increase with increasing strain,
and some of these boundaries may become LAGBs with sucient strain. Ball milling
is a large strain deformation process. The present HREM results indicate that the
grain renement mechanism in the ball-milling process is similar to that proposed
above. In short, it suggests that grain renement during ball milling is a continuous
process that consists of formation of dislocation subboundaries, such as SAGBs in
this case, a gradual rise in the SAGB misorientation due to accumulation of more
dislocations and, nally, the formation of LAGB.
4.2. Non-equilibrium grain boundary
The microstructures developed by cold or high-strain deformation are character-
ized by a relatively high density of dislocation substructures and, therefore, a high
stored energy. Such strain-induced GBs can be in a non-equilibrium state (Horita
et al: 1996, 1998, Huang et al: 2001, Valiev et al: 2000). Non-equilibrium GBs can
lead to changes in fundamental physical and mechanical properties, such as the
elastic moduli, diusion coecient, strength, superplasticity and magnetic properties
of nanostructured materials. Extrinsic dislocations, which are not geometrically
necessary, are frequently observed in cryomilled Cu (such as that shown in gure
7), indicating that the GBs are mostly in non-equilibrium congurations. Similar
non-equilibrium GBs were also found in RCS-processed Cu (Huang et al: 2001) and
in ECAP-processed AlMg (Horita et al: 1996), indicating that non-equilibrium GBs
can exist in nanostructured metals produced by dierent deformation methods. It
should be mentioned that the grain size obtained by ball milling is usually much
smaller than that produced by ECAP or RCS. In the former case, the grain size is
normally less than 100 nm while, in the latter two cases, it is around 500 nm.
} 5. Conclusions
(1) The grain renement during ball milling is a strain-induced continuous
process that consists of formation of dislocation subboundaries, such as
SAGB, a gradual increase in the subboundary misorientation due to
accumulation of more dislocations and, nally, the formation of a LAGB.
(2) The GBs of cryomilled Cu are generally curved, or wavy with non-uniform
contrast, or faceted, which are general features in nanostructured materials.
(3) The GBs in cryomilled Cu are in a high-energy non-equilibrium congura-
tions. The similarity between the cryomilled Cu, room-temperature ball-
milled Cu, ECAP-processed Cu and RCS-processed Cu suggests that non-
equilibrium GBs are typical features of nanostructured metals and alloys
processed using severe plastic deformation techniques.
1418 J. Y. Huang et al.
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ACKNOWLEDGEMENTS
We thank Dr D. W. He for performing the cold compaction of the milled
powders. F. Z. and E. J. L. acknowledge the nancial support from the Oce of
Naval Research under grants N00014-00-1-0109 and N00014-01-1-0882 with Dr
Lawrence Kabaco as program ocer.
References
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GB structure of cryomilled nanocrystalline Cu 1419
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