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Hot Extrusion of Nanostructured Al-Powder Alloys: Grain

Growth Control and the Effect of Process Parameters


on Their Microstructure and Mechanical Properties
A.M. JORGE, Jr., M.M. PERES, J.B. FOGAGNOLO, C.S. KIMINAMI, C. BOLFARINI,
and W.J. BOTTA
Two nanostructured aluminum powder alloys (supersaturated Al4.5Cu prepared by mechanical
alloying, and Al3.0Fe0.42Cu0.37Mn rich in precipitates and prepared by rapid solidication via
gas atomization) were consolidated into bulk material under various processing conditions via
hot extrusion. The microstructural modications and mechanical properties of the consolidated
alloys as a function of the extrusion conditions were investigated and are discussed here. The
eect of pre-existing precipitates from nonsupersaturated alloy is shown to be more eective for
controlling grain growth during consolidation. The increase in the extrusion load, with a concomitant increase in the extrusion rate and decrease in temperature, is shown to lead to
microstructural modications. The dierences in mechanical properties measured by compressive tests are also discussed in association with the extrusion parameters. Furthermore,
suggestions are given for rationalizing the extrusion rate and temperature for the consolidation
of nanostructured aluminum powder alloys via hot extrusion.
DOI: 10.1007/s11661-009-9984-0
 The Minerals, Metals & Materials Society and ASM International 2009

I.

INTRODUCTION

NANOSTRUCTURED materials have been the


subject of extensive research in recent years thanks to
their remarkable potential in terms of physical and
mechanical properties.[14] A variety of techniques, such
as mechanical alloying and rapid solidication, have
been applied successfully to prepare nanostructured
materials.[5] However, when these materials are prepared
by the aforementioned methods, they usually result in
powders or foils that cannot be used directly in
structural applications. Therefore, the development of
consolidation processes suitable for nanostructured
materials, particularly of nanostructured powder materials, is of great interest. Processing powder into a bulk
nanostructured material oers signicant challenges.
The low temperature required to prevent grain growth
limits the processing window (maximum temperature
and time at maximum temperature) to which the powder
can be exposed with modest or no grain growth.
The research published to date has shown that
extrusion is one of the most eective processes for the
consolidation of powder materials.[69] In the present
work, we investigated the inuence of the two main
technical parametersstrain rate and temperatureof
A.M. JORGE, Jr., M.M. PERES, C.S. KIMINAMI,
C. BOLFARINI, and W.J. BOTTA, Professors, are with the
Department of Materials Engineering, Federal University of Sao
Carlos, Rod. Washington Luiz, km 235, 13565-905 Sao Carlos, SP,
Brazil. Contact e-mail: moreira@dema.ufscar.br J.B. FOGAGNOLO,
Professor, is with the Materials Engineering and Science Post
Graduation Program, Sao Francisco University, 13251-900 Itatiba,
SP, Brazil.
Manuscript submitted May 19, 2008.
Article published online September 17, 2009
3314VOLUME 40A, DECEMBER 2009

hot extrusion on the microstructure and mechanical


properties of bulk material consolidated from nanostructured aluminum alloy powder. We have chosen to
study two Al-based compositions due to their importance as structural materials in several applications,
where low density, high mechanical strength, and
corrosion resistance are desirable.

II.

MATERIALS AND METHODS

Rapidly solidied aluminum alloy powder with a


nominal composition of Al-3.0Fe-0.42Cu-0.37Mn
(wt pct) (to be referred to as Al(Fe)), rich in precipitates,
was prepared using argon gas atomization. This procedure resulted in nanostructured aluminum alloy powder
whose microstructure showed an average grain size of
25 nm. The average particle size was 75 lm. Cold
pressing was used to transform the nanostructured
powder into cylindrical preforms with a relative density
of about 0.96 and with an initial diameter of 26.2 mm, in
preparation for consolidation processing. The preforms
were then consolidated into 7.9-mm-diameter bars of
bulk material by hot extrusion at three dierent temperatures, 375 C, 400 C, and 425 C; an extrusion
ratio (ER) of 10:1; and ram speeds (RSs) of 1, 15, and
30 mm/min.
For purposes of comparison, the eect of precipitation on the microstructure and mechanical properties of
the Al(Fe) alloy was compared to that of a supersaturated mechanically alloyed Al-4.5Cu (to be referred to
as Al(Cu)) powder consolidated by hot extrusion under
seven dierent conditions, as follows: ER of 5:1 and RS
of 14 mm/min (at 375 C, 400 C, and 425 C); ER of
METALLURGICAL AND MATERIALS TRANSACTIONS A

10:1, RS of 15 mm/min, and 375 C; and ER of 25:1 and


375 C (at 1, 14, and 30 mm/min). The Al(Cu) alloy was
tested in several conditions to allow the analysis of the
process parameters (ER, RS, and temperature) during
Al2Cu precipitation. All comparisons between the
Al(Fe) and Al(Cu) alloys, with respect of grain size,
were carried out using the same RS (15 mm/min)
guaranteeing the same extrusion time. This powder
was obtained after 10 hours of milling elemental aluminum (gas atomized, purity 99.5 pct) and copper powders
(electrolytic, purity 99.9 pct), in a high-energy ball mill
(ZOZ attritor with container and grinding medium of
stainless steel). More details about this procedure
were published elsewhere.[1] The average mechanically
alloyed particle size was 50 lm. This procedure resulted
in nanostructured supersaturated solid solution of
Al-Cu alloy powders with an average grain size of less
than 50 nm.
The cold pressing and the hot extrusion of both
powders were made without canning, degassing, and
atmosphere control, and were cooled in still air at room
temperature.
The mean extrusion strain rate was calculated by the
following equation:[9]
2
e_ 6VDc tan a2 ln DC
3
DE
DC  D3E

1

where V is the average ram speed, DC is the container


bore (26.2 mm), DE is the diameter of the extruded rod
(7.9 mm), and a is the dead-metal zone semiangle
(60 deg).
The mechanical properties of the bulk material
consolidated from the nanostructured aluminum alloy
powders were determined by means of room-temperature compression tests, which were performed with an
Interactive Instruments 1k-16 universal testing machine
at a compression speed of 0.5 mm/min. The specimens
were machined out in a cylindrical format with a ratio
height/diameter of 2:1, according to the ASTM E 9-89a
specications. Five compression tests were performed

for each extrusion condition. To compare the mechanical properties of both alloys, the mechanical tests were
made in the same conditions and the data concerning
extrusion (ER and RS) were converted to strain rate
using Eq. [1].
The powder alloys and the extruded parts were
characterized by X-ray diraction (XRD) using a
Rigaku diractometer with Cu Ka radiation. Microstructural observations were carried out by transmission
electron microscopy (TEM) using a PHILIPS* CM-120
*PHILIPS is a trademark of FEI Company, Hillsboro, OR.

and a FEI TECNAI G2-F20 microscope. The powders


were ultrasonic dispersed in acetone during 5 minutes
before deposition in a copper grid. Thin foils from the
bulk samples were prepared by ion milling. Before TEM
observation, the specimens were plasma cleaned in
Fischione 1020 equipment, and the energy-dispersive
X-ray (EDX) analysis was performed using a Be lowbackground specimen holder.
The crystallite size and lattice strain were estimated by
measuring the broadening of the X-ray peaks and by
using a modied Scherrer equation and HallWilliamson plot method[10]

III.

RESULTS AND DISCUSSION

A. Grain Size and Microstructure


To evaluate the strength and ductility of the extruded
powder alloys, their microstructures and phase compositions were investigated. The close-up view in Figure 1
shows the XRD pattern after extrusion from samples at
three dierent temperatures.
The peaks observed and identied as fcc-Al solid
solution, Al6Fe, Al2O3, Fe0.9536O, and (FeO)0.664(MnO)0.336
phases can be seen in the XRD pattern from
Figure 1(a). All of them were already present in the

Fig. 1XRD patterns of the bulk of the powder alloys after extrusion: (a) Al(Fe) and (b) Al(Cu).
METALLURGICAL AND MATERIALS TRANSACTIONS A

VOLUME 40A, DECEMBER 20093315

initial powder and formed during argon gas atomization


processing. In the Al-Fe system, a eutectic with composition between 1.7 and 2.2 pct Fe is formed at 655 C.
The equilibrium phase with aluminum is Al3Fe (40.7 pct
Fe), although it can approach Al7Fe2 (37.3 pct Fe). The
phase Al3Fe is formed starting from the liquid, already
at 1150 C, and not from the peritectic reaction. When
the specimen is rapidly quenched, the metastable phase
Al6Fe (22.6 pct Fe) is formed.[11]
Figure 1(b) also shows two phases, fcc-Al solid
solution and Al2Cu, but the latter was not found in
the initial powder and in the sample extruded at 425 C.
In both cases, it is relevant to note the considerable
reduction in the width of the fcc-Al peak with increasing
extrusion temperature, indicating the predominance of
nanosized fcc-Al grains in the initial powder. This eect
is more pronounced in the Al(Cu) alloy, suggesting more
extensive grain growth. Also visible is the contraction
and reduction of intensity of the metastable Al6Fe peak
with rising extrusion temperature, indicating both precipitate coarsening and dynamic dissolution. In spite of
the low solubility of the Fe in Al, matrix dissolution of
Al6Fe in the aluminum matrix has already been both
observed to occur by eutectoid decomposition of the
crystalline Al6Fe into equilibrium phases[11] and induced
by deformation in this case with the formation of an
Al-Fe solid solution, Al9Fe2 and Al5Fe2 aluminides,
and their defective modications.[12] In our samples, the
amount of aluminide particles is expected to be very
small, justifying that we could not detect them by XRD;
the results from TEM analysis will be discussed later. In
the case of the Al(Cu), the width as well as the intensity
of the Al2Cu peak is also reduced, indicating coarsening
and dissolution of the precipitates.
Figure 2 shows the average grain size of the bulk
aluminum alloys before and after extrusion as a function
of extrusion temperature. The value at 25 C is the
powders average grain size. The data points were tted
to a representative curve to identify the approximate
behavior between 25 C and the other temperatures. It is
believed that there is a critical temperature for grain
growth during consolidation by hot extrusion. When the
extrusion temperature exceeds the critical one, the
average grain size of the consolidated alloy quickly
increases along with the rising extrusion temperature,

reaching about 70 nm for the Al(Fe) alloy and 840 nm


for the Al(Cu) alloy at 425 C. The inuence of the
process parameters on the Al2Cu precipitation was
analyzed. The worst case was 1 mm/min, with the grain
size reaching almost 2 lm. In 30 mm/min, the changes
in grain size were negligible when compared with
15 mm/min. The extrusion ratio had no eect on the
precipitation.
Grain growth kinetics for a number of materials has
been reviewed and studied.[1319] Grain growth occurring at low values of T/TM (where TM stands for melting
point of the material) might indicate abnormal grain
growth at grain boundaries in a less inhibited manner.[14] In this case, the apparent activation energy of
grain growth was compared to the activation energy for
grain boundary and lattice diusion. In hot working
conditions (T/TM > 0.5), particle pinning, solute drag,
and reduction in grain boundary energy were proposed
as grain size stabilization mechanisms.[15] Some
authors[18] have provided a qualitative description to
validate the incorporation of grain boundary energy
into the grain growth kinetics.
If one considers the grain growth of the nanostructured aluminum alloy during hot extrusion as isothermal
grain growth, then the grain growth behavior depends
mainly on two factors that govern the grain growth rate,
i.e., the apparent activation energy (Q) and the extrusion
temperature (T). Apparent activation energies for grain
coarsening are generally dicult to assess. Malow and
Koch[20] compiled the existing apparent activation
energy data for grain coarsening in consolidated nanosize metals. Since nanosize grains usually have very high
apparent activation energy for grain growth,[20] the
grain growth rate has a tendency to be lower when the
nanostructured aluminum alloy powder undergoes hot
extrusion at relatively low temperatures. As a result, the
grain growth is not expected to be signicant when the
extrusion temperature is low, and contrary to expectations,[21] grain growth in nanocrystalline materials,
prepared by any method, is very small up to a
reasonably high temperature.[21] If the apparent activation energy is unchanged, raising the extrusion temperature will increase and accelerate the grain growth
rate. In fact, when the extrusion process is performed
within a relatively low-temperature range, the apparent

Fig. 2Dependence of the average grain size on extrusion temperature: (a) Al(Fe) and (b) Al(Cu) compared with A(Fe).
3316VOLUME 40A, DECEMBER 2009

METALLURGICAL AND MATERIALS TRANSACTIONS A

activation energy of the nanostructured aluminum alloy


will increase with rising temperature due to the precipitation eect that pins the grain boundary movement
necessary for grain growth. Therefore, when extrusion is
carried out at temperatures below the critical one, the
grain growth rate can be kept relatively low and is
expected to be limited to a certain amount. However,
when the temperature rises to the critical value, the
precipitates coarsen and dissolve, leading to the reduction or disappearance of their pinning eect and thus
decreasing the apparent activation energy, even as the
eect of increasing temperature on enhancement of the
grain growth rate becomes more important. Therefore,
when the extrusion process is carried out at temperatures above the critical value, grain growth increases
very rapidly.
Figure 2 indicates that the behavior of the two
materials is the same and is congruous with the
preceding discussion, but there is a remarkable dierence in the grain growth rate of the alloys. The initial
state of the two alloys is quite dierent, i.e., Al(Cu) is
highly deformed and free of precipitates, with all the Cu
particles in solution, while the Al(Fe) is free of deformation and precipitate rich. When the temperature is
increased, the precipitates in Al(Fe) start to pin the
grain boundary eectively, but the particles responsible for boundary pinning in Al(Cu) are absent and have
to follow the sequence of Cu precipitation during
processing.
Grain growth in Al(Cu) begins around 200 C[1,22,23]
and progresses with increasing temperature.[1,22,23] At
the same time, copper segregates at the grain boundaries
and dislocations.[24] The phase sequence and microstructure of Al(Cu) have been studied extensively.[22,2527]
The following sequence of structures is observed when
annealing the supersaturated solid solution: Guinier
Preston (GP) zones, GP1, GP2 (also called h), h, and h
(Al2Cu).[28] The density of precipitates is not determined
by the amount of Cu but related to the density of
nucleation sites for precipitation.[24] Additionally, in
Al(Cu) powders, the formation of h is generally not
observed.[25] In this context, before the highly deformed
particles (from mechanical alloying) begin to deform in
extrusion, there is no precipitation and the grains grow.
During the Al(Cu) powder milling, a large increase in
the density of dislocation occurs. The Cu segregates to
interfaces and distorted regions, resulting in a smaller
amount of Cu in solution.[29] The dislocations, competing with the grain boundaries, are slightly compressed.
The associated distortion energy at such lattice sites may
be minimized by replacing the solvent atom (here Al)
with the smaller (Cu) solute atom.[29] Doing that would
cause the Cu atoms to diuse to the slightly compressed
sites. Such preferred segregation would lower the driving
force for nucleation in other sites, because the amount
of Cu in solid solution would be smaller. During hot
extrusion, once the second-phase particles nucleated,
they would, in this case, grow preferentially along the
dislocation lines inside the grains instead of at the grain
boundaries, avoiding the grain boundary pinning eect
and allowing an extended grain growth in Al(Cu)
powders.
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 3Bright-eld TEM images: (a) and (b) powders, (c) Al(Fe)
bulk aluminum alloy consolidated at 425 C, and (d) Al(Cu) bulk
aluminum alloy consolidated at 375 C. (Magnications: (a) 230 K,
(b) 88 K, (c) 175 K, and (d) 110 K.)

Figures 3(a) (Al(Fe)) and 3(b) (Al(Cu)) show TEM


images of the aluminum powder alloys and the selected
area electron diraction pattern (SAEDP), showing the
fcc-Al pattern and the small grain dimensions (25 nm
for Al(Fe) and 50 nm for Al(Cu)). Figure 3(a) also
reveals the presence of small precipitates, especially at
grain boundaries, indexed, in the respective SAEDPs, as
Al6Fe, which is in agreement with the results in
Figure 1(a). This gure also indicates that the sizes of
Al6Fe intermetallic precipitates are similar to those of
the fcc-Al, which are on average about 25 nm, and that
the volume fraction of these precipitates is about 8 pct.
Figure 3(b) shows no obvious precipitation, in accordance with Figure 1(b).
Figures 3(c) (Al(Fe)) and 3(d) (Al(Cu)) show brighteld TEM images of the as-extruded bulk aluminum
alloy consolidated from nanostructured powder at
425 C and 29.3 s1 and at 375 C and 20 s1, respectively. The grain sizes in these TEM images appear to be
congruous with the results of the XRD analysis shown
in Figures 2(a) and (b), respectively.
VOLUME 40A, DECEMBER 20093317

of the alloying elements in aluminum at the nal


temperature (which is congruent with the XRD pattern
shown in Figure 1). Obviously, the TEM results support
the preceding analysis for the grain growth of these
nanostructured aluminum alloys during the extrusion
process.
B. Mechanical Properties

Fig. 4Al(Fe) bulk aluminum alloy consolidated at 425 C: (a)


bright-eld TEM, image; (b) bright-eld STEM image, showing very
small precipitates (white arrowhead); and (c) EDX spectra obtained
from precipitate (+1) and matrix (+2) observed in (b). (Magnications: (a) 550 K and (b) 1.8 M.)

Figure 4 shows the results of TEM observations for


the (Al(Fe)) sample consolidated at 425 C. The presence of very small precipitates can be seen in the TEM
and scanning transmission electron microscopy (STEM)
bright-eld images of Figures 4(a) and (b), respectively.
Figure 4(c) shows EDX spectra obtained from the
precipitate (+1) and matrix (+2) of the as-extruded bulk
aluminum alloy consolidated at the same condition of
Figure 3(c).
The main microstructural features depicted in
Figures 3(c) and 3(d) and Figure 4 are as follows. (1)
Figure 3(c), which corresponds to the nal extrusion
temperatures, reveals no obvious particle precipitation
in the consolidated bulk material, only in the powder
before extrusion (Figure 3(a)); however, in Figure 4, one
can see the presence of precipitates, ranging from 3 to
13 nm, and that they are smaller than those observed in
the original powder (Figure 3(a)). Figure 4(c) shows the
presence of iron in the Al matrix. As commented earlier,
these two features are in agreement with other results
reported in the literature, i.e., deformation-induced
eutectoid decomposition of the crystalline Al6Fe into
equilibrium phases[11] decreasing the precipitate particle
size with the formation of an Al-Fe solid solution.[12] (2)
Figure 3(d), which corresponds to the initial extrusion
temperatures, shows the typical SAEDP for the
observed particles, showing an [011] zone of Al (white
squares) superimposed to the Al2Cu [011] axis zone, and
that the preferential sites for the nucleation of these
precipitates was intragranular, as mentioned earlier
herein, with a few precipitates pinning grain boundaries.
(3) In both cases, the quantity of precipitated particles
was signicantly reduced, indicating dissolution of the
precipitate and signicant enhancement of the solubility
3318VOLUME 40A, DECEMBER 2009

Figure 5 shows the dependence of the compressive


mechanical properties of the as-extruded alloys at room
temperature on the extrusion temperature. The ductility
of the as-extruded Al(Fe) alloy (Figure 5(a)) tends to
increase along with rising extrusion temperature. Also,
the ductility of the consolidated material increased
signicantly only within the range of 375 C to 400 C.
A slight decrease in ductility with rising temperature was
observed at higher temperatures (400 C to 425 C).
Because the ductility of the bulk material consolidated
from powders is extremely dependent on the densication eects of the powder preform and on the bonding
condition of the powders, it is believed that good
properties can only be obtained for the consolidated
nanostructured aluminum powder when the extrusion
temperature is around 400 C. For the Al(Cu) alloy
(Figure 5(b)), the dierence was remarkable; i.e., the
ductility started at practically the same values as for
Al(Fe), but decreased with increasing temperature,
probably due to the embrittling eect of the Al2Cu
precipitates, in spite of the grain size in Al(Cu) alloy. The
compressive steady-state strength, rss, showed a similar
dependence on the extrusion temperature. When the
nanostructured aluminum alloy powders were extruded
at temperatures below 400 C, the consolidated material
had a reasonably high strength despite the poor bonding
of the powder particles, because grain growth during
extrusion was minor (Al(Fe)) and also due to the
hardening eect (stronger in the Al(Cu) alloy) produced
by the existing precipitates. However, when the extrusion
process was performed within the temperature range of
375 C to 400 C, the strength of the consolidated
material was considerably reduced. This may have
resulted from the breakdown of cohesion between the
precipitates and the matrix lattice, and coarsening of the
precipitates, leading to the disappearance or reduction of
precipitation hardening and to signicant grain growth
in the Al(Cu) alloy. The bonding condition of the
powders could not be enhanced signicantly within
the temperature range of 375 C to 400 C. When the
extrusion temperature was increased to the range of
400 C to 425 C, the strength of the consolidated
material strength tended to increase again due to the
signicant strengthening of the powder bonding condition and to the increase in the solubility of the alloy
elements in the matrix lattice, even considering the grain
growth that occurred during the extrusion process.
These results suggest that to obtain both high strength
and good ductility, the hot extrusion temperature of
these nanostructured aluminum powders should be
selected within the range of 400 C to 425 C for Al(Fe)
and at around 380 C for Al(Cu). At extrusion temperatures of more than 425 C, the strength of the
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 5Dependence of the compressive mechanical properties at room temperature on the extrusion temperature: (a) and (c) Al(Fe) and (b) and
(d) Al(Cu), compressive strain and compressive steady-state stress, respectively.

consolidated material decreases as the temperature


increases due to excessive grain growth.
Figure 6 shows the dependence of the compressive
mechanical properties of the as-extruded alloys at room
temperature on the extrusion strain rate in the entire
extrusion temperature range. Note that both the compressive strength and ductility of the as-extruded alloy
increase as the strain rate increases. Increasing the strain
rate increases the pressure and the shear deformation
that the powders undergo during extrusion, heightening
the densication eect of the bonded powder. At
extrusion strain rates exceeding 14.7 s1, the mechanical
properties of the as-extruded alloy do not improve
noticeably, and they decrease in the Al(Cu) alloy at
strain rates above 29 s1. This suggests that an extrusion
rate of 14.7 s1 can ensure good bonding strength and
full densication of the powder material. Therefore, the
appropriate strain rate for the hot extrusion of nanostructured aluminum powders lies within the range of
14.7 to 29 s1. On the other hand, a very high strain rate
raises the cost of the process, without producing
any substantial increase in the materials mechanical
properties.
METALLURGICAL AND MATERIALS TRANSACTIONS A

IV.

CONCLUSIONS

1. X-ray diraction experiments showed a precipitation onset temperature during heating of Al(Cu)
alloy. Second-phase particles were identied as the
stable incoherent Al2Cu phase.
2. Intermediate phase transformations, such as those
often found upon heating bulk Al-Cu, were not
observed here. The Cu is believed to segregate preferentially in dislocations, due to the powders high
dislocation density not totally eliminated during
heating, which increased after straining. Secondphase particle formation starts when these sites are
saturated.
3. The eect of the pre-existing precipitates from
Al(Fe) alloy was shown to be more eective in controlling grain growth than that of supersaturated
Al(Cu), due to the preferential intragranular nucleation sites that promoted unpinning of grain
boundaries in the Al(Cu) alloy.
4. The bonding strength of the nanostructured
aluminum powder was susceptible to the extrusion
temperature.
VOLUME 40A, DECEMBER 20093319

Fig. 6Dependence of the compressive mechanical properties at room temperature on strain rate: (a) and (c) Al(Fe) and (b) and (d) Al(Cu),
compressive steady-state stress and compressive strain, respectively.

5. A higher extrusion rate proved useful to increase


the powder bonding strength and the densication
eect, enhancing both the ductility and the compressive strength of the consolidated material.
ACKNOWLEDGMENTS
The authors gratefully acknowledge the Brazilian
research funding agencies CNPq and FAPESP for
their support of this work.

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