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Pure metal microspecimens have been found to exhibit strong size dependence of strength, but alloyed counterparts with a much
rened microstructural length scale due to the precipitates present are as yet unknown. Here, compression tests on duralumin (aluminum 2025 alloy) micropillars reveal a much weaker size dependence of strength compared to pure Al, indicating the predominance
of the internal length scale in determining strength. Creep is also signicant in duralumin, probably due to the viscous overcoming of
obstacles during deformation.
2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Plastic deformation; Compression tests; Dislocations; Nanoindentation; Precipitation hardening
The strength of micron-sized metallic single crystals has been found to depend on their size generally in
accordance with a power law [13], with jerky stress
strain behavior [1,48]. Such unusual deformation behavior is now explainable by a number of mechanisms which
have received direct experimental support [8,9]. The dislocation starvation [6] theory considers that small crystals can remain in a dislocation-free state as the mobile
dislocations glide and are eliminated at free surfaces without accumulation and multiplication. The source truncation [10] and exhaustion hardening [11] models
consider the distribution and operation of dislocation
sources in a small conned volume, leading to the breakdown of a mean-eld condition for forest hardening. The
power law dependence of the strength on size has also
been explicitly predicted as a consequence of Taylor-type
hardening in an initial fractal dislocation network [12].
While the jerky deformation of monolithic microcrystals is due to the ease of loss of dislocations from the
specimen volume, several studies have investigated
methods to trap dislocations inside the specimen, such
as coating its surface [13,14]. Experiments on microsized
bicrystals have also shown improved strengthening and
suppressed serrated ow when compared with the single
crystalline state [15], but in nanosized bicrystals, the
grain boundary could act as a dislocation sink, leading
to adverse eects [16]. The deformation behavior of micro- and nanospecimens with polycrystalline [17] and
even nanocrystalline [1820] substructures has also been
1359-6462/$ - see front matter 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.scriptamat.2013.02.012
862
Figure 1. Stressstrain curves of micropillars of dierent sizes fabricated from an [0 1 1] grain on (a) RT-aged and (b) peak-aged
duralumin alloy, respectively.
The microstructures in the 10 1% deformed duralumin micropillars aged at RT and under peak conditions
with dierent sizes are shown in Figure 4(ae). Here, the
TEM images were taken with diraction vectors g under
which visible dislocations were most abundant. Figure 4(a) shows that the dislocations in an RT-aged 1 lm
pillar distributed inhomogeneously within the specimen.
In some regions they were entangled together with density
up to 1 1015 m2 as measured by a line-intercept
method [14], as shown in Figure 4(b), while in other regions, such as a slip band, the dislocation density was
much lower, indicating that a lot of the dislocations had
escaped from the pillar. Large dispersoids are also visible
as dark round spots with sizes in the submicron range. In
the typical TEM image of an RT-aged 5 lm pillar shown
in Figure 4(c), the dislocation distribution is similar to
that in the 1 lm pillar shown in Figure 4(b). However,
for the peak-aged pillars in Figure 4(d and e), the size effect on the dislocation distribution is more signicant
the dislocation density in the 1 lm pillar in Figure 4(d)
is 1 1014 m2, which is signicantly smaller than the
2 1015 m2 in the 5 lm pillar in Figure 4(e).
Recent research [2427] has revealed that, in an Al
CuMg alloy, the rst stage of hardening after the water
quench is due to the formation of CuMg co-clusters at
low temperature, and after articial aging a hardness
plateau is reached when the S phase and GuinierPrestonBagaryatsky (GPB) zones co-exist, with the S phase
(Al2CuMg) being the major strengthening precipitate,
while the rod-shaped dispersoids of T phase (Al20Cu2Mn3) commonly found in duralumin do not make a
signicant contribution towards hardening. In the
peak-aged state the lath-shaped S precipitates have submicron size and spacing [24,25], which are much larger
than the nanometer-sized co-clusters and GPB zones
produced during RT aging [25].
Figure 2 shows that the 2% proof strength of duralumin
micropillars decreases with size in te power law r / Dm ,
with m 0.34 and 0.51 for the RT-aged and peak-aged
states, respectively. The value of m for duralumin pillars
here is therefore similar to that in pure Al pillars with sig-
Figure 4. (a) TEM montage of a longitudinal section of an 1 lm RTaged pillar. (b, c) High-magnication bright-eld images of RT-aged
pillars of 1 and 5 lm diameter, respectively. (d, e) High-magnication bright-eld images of peak-aged pillars of 1 and 5 lm
diameter, respectively. All pillars were deformed to 10 1%.
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The dislocation densities at 10 1% deformation observed from Figure 4 also correspond to the 10% ow
stresses in Figure 2 rather well, in that the 1 lm peak-aged
pillars exhibit the greatest strength while the 5 lm peakaged pillars exhibit the least strength, and the strength of
the RT-aged pillars is in-between, with almost no size
dependence. The 1 lm peak-aged pillars are strongest because of the partial loss of dislocations to the free surface,
i.e. according to the Orowan equation e_ qbv, the mobile
dislocation density is continuously lower so that a higher
stress is needed to make the limited quantity of mobile dislocations travel faster so as to maintain a given strain rate.
On the other hand, the larger 5 lm peak-aged pillars are
the weakest because more dislocations are now retained
inside the pillar by the precipitates, and the RT-aged pillars are of intermediate strength because of the intermediate capability of the nanoscale precipitates to retain
dislocations. As mentioned above, this inverse trend of
dislocation density vs. strength tallies well with the Orowan equation, but is notpconsistent
with Taylors work
hardening rule of r / q, suggesting that strength in
duralumin pillars is not controlled by mutual dislocation
interactions but by dislocation drag by precipitates. This
phenomenon is analogous to a previous observation
[12,14] that pre-straining can produce softening in small
(1 lm) Al pillars the pre-straining in that case increases
the mobile dislocation density, so there are now more carriers for slip.
It is also interesting to see from Figure 2 that the 2%
proof strength of the 5 lm pillars in the peak-aged condition is substantially lower than that in the RT-aged condition, but this dierence narrows down tremendously for
the 10% ow stress. In fact, even in the peak-aged state,
the bulk hardness (125 Hv) is only marginally higher
than that in the RT-aged state (110 Hv) and, since the
Vickers hardness scale is a measure of the ow stress up
to 7% strain [30], the bulk hardness should better be
compared with the 10% ow stress data than the 2% proof
stress data in Figure 2. Assuming the Vickers hardness is
3.3 times the ow strength, as is typical for hardening
materials, the bulk ow strength should therefore be 387
and 333 MPa for the peak-aged and RT-aged states of
the present duralumin, respectively, and these values are
comparable with the 10% ow stress of the 5 lm pillars
in Figure 2. The strength of the bulk state should be controlled by long-range undulations in the distribution of
the precipitates which are not present in the micron-sized
pillars, though further work is necessary to clarify the relationship between the strengths of micron-sized samples
and bulk samples.
Another remarkable observation is that signicant
creep occurs in duralumin micropillars but not in pure
aluminum pillars [7,12,14]. This is likely to be due to
the various obstacles for dislocation motion in duralumin which are not present in pure aluminum, including
interactions with precipitates and solute drag. These
obstacles are bypassed by thermal uctuations and/or
climb of the dislocations and, as a result, the resultant
deformation has a signicant viscous character. Again,
the creep behavior of microsized alloys warrants further
investigation.
To conclude, precipitate-hardened duralumin alloy
pillars exhibit a power law (r / Dm ) size dependence