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DOI 10.1007/s10853-014-8099-1
Received: 29 November 2013 / Accepted: 31 January 2014 / Published online: 15 February 2014
Springer Science+Business Media New York 2014
Introduction
Many past papers have reviewed the effect of grain size on
the mechanical properties of nanocrystalline metals (e.g.,
[13]). As per the HallPetch grain size hardening mechanism, nanometals exhibited significant increases in yield
strength and hardness (e.g., [46]). However, limited tensile ductility was usually observed for nanocrystalline
materials in comparison with their conventional coarsegrained counterparts due to their low capacity for strain
hardening [2, 7]. Low tensile ductility of nanomaterials is
almost invariably associated with early onset of localized
deformation, e.g., necking and/or shear bands [811].
While a great deal of effort has focused on the underlying
deformation mechanisms (e.g., [1217]), there is limited
experimental investigation on the phenomena of localized
strain and heat generation during plastic deformation of
these materials, which could have a significant effect on the
microstructure and mechanical properties [18].
There is considerable debate over the possibility of
thermally activated grain growth due to heat generation
associated with localized strain of specimens during deformation. Previous studies have reported grain growth during
tensile testing in nanocrystalline Ni [10], NiFe [18] and
CoP [19], all produced by Integrans electrodeposition
process [2022]. For example, nanocrystalline Ni (grain
size: 20 nm) was tested in tension at strain rates between
10-5 and 10-1/s [10]. Transmission electron microscopy in
one of the shear band regions at the higher strain rates
revealed considerable grain growth. It was speculated that
grain growth in nanocrystalline Ni was due to the kinetic
energy released during high-speed deformation, which
could result in local hot spots within the shear band reaching
temperatures on the order of 300 C [10]. At this temperature, significant grain growth is expected to take place in the
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Experimental
The materials used in this study consist of four batches of
samples, coarse-grained polycrystalline nickel (commercially
available Ni 200), and three nanocrystalline electrodeposits,
Ni and two NiFe alloys with different Fe contents. All
nanocrystalline electrodeposits were prepared by Integran
Technologies Inc, which used the same process to produce
the samples for the investigations in Refs. [10, 18, 19].
Samples from the same nanocrystalline batches were already
characterized in previous studies [25, 26], using transmission
electron microscopy and X-ray line broadening measurements (Scherrer approach) [27], as well as energy-dispersive
X-ray spectroscopy (EDS). For the polycrystalline Ni, the
grain size was determined using standard metallography.
Tensile coupons of 1.0 mm thickness were machined by
the electric discharge machining (EDM) method to produce
dog-bone-shape tensile testing samples with dimension
details as shown in Fig. 1. There was a minor modification in
the geometry of tensile coupons in the current study with
respect to ASTM E8 standard. The coupon tab width was
widened from 10 to 20 mm (Fig. 1) to provide increased
gripping area after slipping problems owing to the extremely
high material strength were experienced, while the rest,
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3849
Fe content
(wt%)
Average
grain size
32 lm
2. Nanocrystalline Ni
23 nm
3. Nanocrystalline NiFe 1
2.6
16 nm
4. Nanocrystalline NiFe 2
8.5
16 nm
grain size of 23 nm, while the two NiFe samples both had
a grain size of 16 nm as per XRD line broadening measurements [25, 26].
Deformation at different tensile strain rates
All materials were tested at strain rates of 10-1 and 10-2/s.
Figure 2 shows the respective engineering stressstrain
curves for all samples.
At the rate of 10-2/s, the coarse-grained Ni (grain size:
32 lm) showed a yield strength (YS) of 208 MPa, ultimate
tensile strength (UTS) of 442 MPa and considerable ductility with total elongation (or total global strain) of 50.4 %.
With the refinement of grain sizes, there is a significant
increase in YS and UTS due to the HallPetch grain size
strengthening mechanism as indicated in Fig. 2a. The
nanocrystalline Ni (grain size: 23 nm) showed values of
YS (950 MPa) and UTS (1504 MPa), about 4 times higher
than the coarse-grained Ni. The two remaining 16 nm
NiFe samples exhibited different strength values, YS of
1010 and 1130 MPa, as well as UTS of 1579 and 1741 MPa,
for the Ni-2.6 wt% Fe and Ni-8.5 wt% Fe, respectively. The
fact that higher strength was observed at higher Fe content
suggests that there is some solution-strengthening effect due
to Fe solute for the NiFe samples. In addition, all
Fig. 2 Stress-strain curves of all samples deformed at a strain rate of a 10-2/s and b 10-1/s
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3850
Grain size
Strain
rate (/s)
Poly-Ni
32 lm
10-2
208
-1
10
10-2
Nano-Ni
Nano-Ni-2.6 % Fe
Nano-Ni-8.5 % Fe
23 nm
16 nm
16 nm
Elongation
at UTS (%)
Total
elongation (%)
442
45
50.4
208
445
45
51
950
1504
5.5
8.2
10-1
970
1508
5.5
10-2
1010
1579
5.5
7.6
10-1
1100
1763
5.5
7.5
-2
1130
1150
1741
1867
5.5
5.5
7.7
7.5
10
10-1
Yield strength
(MPa)
123
UTS
(MPa)
3851
(a)
(b)
Poly Ni (0.1/s)
50%
80
45%
35%
25%
15%
Local strain, %
60
Region 1
Region 2
Region 1
40
20
0
0
10
20
30
40
Gauge length, mm
Fig. 3 Strain distribution at different global strains for the coarsegrained Ni (grain size: 32 lm), a strain field contour maps, and
b strain distributions within the gauge length at five levels of global
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3852
(a)
15
(b)
Nano Ni (0.1/s)
7.5%
5.5%
4.5%
12
3.5%
Local strain, %
2.5%
Region 1
Region 1
Region 2
0
0
10
15
20
25
30
35
40
Gauge length, mm
Fig. 4 Strain distribution at different global strains for the nanocrystalline Ni (grain size: 23 nm), a strain field contour maps, and b strain
distributions within the gauge length. Region 2 is approximately located between the two red-dotted lines (Color figure online)
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3853
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Fig. 5 Temperature change in
coarse-grained Ni, a infrared
images with the dashed line at
50 % strain indicating the final
fracture position, and
b engineering stressstrain
curve and the maximum
temperature increase, DTmax, at
a strain rate of 10-1/s. Note that
the numbers on the color scale
bar are temperature in Celsius
(Color figure online)
(a)
550
500
450
400
350
300
250
200
80
500
(b)
400
u
300
40
200
0
Tmax , C
60
20
100
0
0
10
20
30
40
50
60
Global strain/Elongation, %
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3855
(a)
600
550
500
450
400
350
300
250
200
70
1600
(b)
1200
50
40
800
30
0
Tmax , C
60
20
400
10
0
0
0
Global strain/Elongation, %
Poly-Ni
Nano-Ni
Nano-Ni-2.6 % Fe
Nano-Ni-8.5 % Fe
Grain
size
Strain
rate (/s)
32 lm
23 nm
16 nm
16 nm
Tmax
(C)
Total
At UTS
10-2
50.4
45
50
10-1
51
45
95
10-2
8.2
5.5
59
10-1
5.5
83
10-2
7.6
5.5
57
10-1
7.5
5.5
79
-2
10
7.7
5.5
59
10-1
7.5
5.5
81
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3856
reported onset temperatures for the initiation of microstructure evolution, e.g., by subgrain coalescence, for
20 nm grain size Ni electrodeposits [24]. Moreover, the
highest measured Tmax value was approximately 80 C for
the two nanocrystalline NiFe samples, while their grain
growth temperature was reported to be 50100 C higher
than that of the nanocrystalline Ni due to the stabilizing
effect of the alloying element Fe (e.g., [23]). Evidently
based on the measured Tmax alone, the strain-induced heat
release is likely not sufficient to activate migration of grain
boundaries.
One uncertainty regarding the measurement of Tmax is the
spatial resolution of the infrared camera. As shown in Ref.
[10], grain growth during tensile testing may be confined in
a narrow band area less than half a micrometer across. It is
unlikely that the infrared camera with a spatial resolution of
about 50 lm used in the current study can detect temperature differences within a submicron area; the measured Tmax
was actually an average value over a larger area. It is possible that a small area in the deformation core attained an
instant local temperature higher than the measured Tmax
during the tests. The temperature difference between the
maximum and minimum value in the resolution unit area,
DTRes, may be estimated using a 1D heat conduction model,
defined by Fouriers law, along the cross-section normal,
DQ
DT
jA
Dt
Dx
qcp L2
b
2j
123
Summary
Temperature increases were measured during tensile testing of both coarse-grained Ni and nanocrystalline Ni and
NiFe electrodeposits due to strain-induced heat generation. Generally, higher strain values and/or higher strain
rates resulted in higher observed peak temperature for each
material, with the highest temperatures recorded in the
regions of subsequent fracture. For the coarse-grained
polycrystalline Ni, the maximum attained mechanically
induced temperature was approximately 95 C, whereas
the highest temperature for the nanocrystalline electrodeposits was approximately 83 C. This is significantly below
the reported threshold temperatures for the onset of thermally activated grain growth in nanocrystalline Ni and
NiFe alloys. Therefore, thermally activated grain growth
is highly unlikely for nanocrystalline Ni and NiFe during
room temperature tensile testing. Previously reported grain
growth events observed in similar materials are likely due
to stress-driven grain boundary migration.
3857
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