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J Mater Sci (2014) 49:38473859

DOI 10.1007/s10853-014-8099-1

Localized strain and heat generation during plastic deformation


in nanocrystalline Ni and NiFe
T. Chan Y. Zhou I. Brooks G. Palumbo
U. Erb

Received: 29 November 2013 / Accepted: 31 January 2014 / Published online: 15 February 2014
 Springer Science+Business Media New York 2014

Abstract Room temperature tensile testing was performed


on a coarse-grained polycrystalline Ni (32 lm), a nanocrystalline Ni (23 nm) and two nanocrystalline NiFe (16 nm)
electrodeposits at two strain rates of 10-1 and 10-2/s. Strain
localizations and local temperature increases were simultaneously recorded during tensile testing. For all materials,
higher loads or higher strain rate generally resulted in higher
peak temperature with the highest temperatures recorded in
the fracture regions. The maximum temperature for the
nanocrystalline materials was just over 80 C, which is significantly below the reported temperatures for the onset of
thermally activated grain growth. Therefore, the previously
reported grain growth observed on similar materials after
tensile deformation is likely not thermally activated but a
stress-induced phenomenon. Despite the wide grain range
from 16 nm to 32 lm, all samples exhibited similar strain
localization behavior. Local strain variations initiated in the
early stage of macroscopic uniform deformation, subsequent
necking and fracture took place in the region of initial strain
localization. While the coarse-grained polycrystalline Ni
exhibited little strain rate sensitivity, gradually increased
strain rate sensitivity was observed for the 23 nm Ni and the
two 16 nm NiFe samples, suggesting that both dislocationmediated and grain-boundary-controlled mechanisms were
operative in the deformation of the nanocrystalline Ni and
NiFe samples.
T. Chan  Y. Zhou (&)  U. Erb
Department of Materials Science and Engineering,
University of Toronto, 184 College Street, Suite 177,
Toronto, ON M5S 3E4, Canada
e-mail: yijian.zhou@utoronto.ca
I. Brooks  G. Palumbo
Integran Technologies Inc, 6300 Northam Drive,
Mississauga, ON L4V 1H7, Canada

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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20 nm Ni electrodeposits. Calorimetric studies have shown


that peak growth temperatures for major grain growth are in
the range from 280 to 290 C for the Ni electrodeposits with
average as-deposited grain size between 15 and 30 nm [23].
Moreover, grain growth activity was observed in a sequence
of relaxation and subgrain coalescence processes when
20 nm Ni electrodeposits were subjected to annealing at
lower temperatures, as low as 120 C [24]. Higher thermal
stability was observed in nanocrystalline NiFe. For
example, the Ni-10 wt% Fe (grain size 15 nm) and
Ni-20 wt% Fe (grain size 13 nm) displayed peak temperatures of grain growth around 334 and 379 C, respectively,
indicating a stabilizing effect by alloying nanocrystalline Ni
electrodeposits with Fe [23]. These experimental observations provide a basis to assess the possibility of having
potential grain growth resulting from localized heating in
nanocrystalline nickel-based electrodeposits during room
temperature deformation.
The main focus of the current study was (1) to establish
a correlation between localized strain and heating, and (2)
to assess the possibility of having thermally activated grain
growth in this type of nanomaterials. Heat dissipation and
strain localization during in situ tensile testing at different
strain rates were investigated on nanocrystalline Ni and
NiFe electrodeposits produced through the same production facility and using the same synthesis process as those
for the samples used in Refs. [10, 18, 19].

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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J Mater Sci (2014) 49:38473859

Fig. 1 Tensile coupon dimensions in mm

especially the critical gauge section, was kept identical to that


of ASTM E8.
All materials were tested at tensile strain rates of 10-2
and 10-1/s on a MTS servo-hydraulic testing machine
combined with the in situ measurements of local strain and
temperature across the gauge length, using the digital
image correlation (DIC) technique and an infrared camera,
respectively. Prior to tensile testing, each sample was
prepared by spraying a layer of black paint on one side to
equalize emissivity for better infrared detection, thus more
accurate temperature measurement. On the opposite side,
samples were lightly abraded using 320 silicon carbide
paper for the measurement of localized strains. Localized
strain patterns during deformation were captured by a high
resolution DIC Camera (Allied Vision Technologies),
while the global strain was obtained based on the crosshead
displacement of the MTS machine frame. Samples with
abraded surfaces facing toward the CCD camera were
illuminated by a source of white light during the entire
tensile testing. The images were post-processed through a
DIC system to calculate the displacement and the localized
strain distributions. Localized strains contours were then
mapped along the sample gauge over a length of 40 mm.
Changes of temperature in the samples were measured
using a pre-calibrated high resolution infrared camera
(Deltatherm 1410) during tensile deformation. Frame rates
of the infrared detector were set to 15 frames per second to
best capture the temperature profiles along sample gauges.
Images captured during the experiment were post-processed through a Thermoelastic Stress Analysis (TSA)
system to locate the temperature increase along the gauge
section during tensile testing. The maximum temperature
along the sample gauges was recorded for all samples.

Results and discussion


Grain size and chemical composition
Table 1 summarizes the chemical compositions and grain
sizes for the samples used in the current study. For the
coarse-grained Ni, i.e., commercial Ni 200, the average
grain size of 32 lm was obtained after analysis of a series
of optical micrographs and measurement of over 400
grains. For the nanocrystalline materials, the nano-Ni had a

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Table 1 Sample grain size and composition


Sample

Fe content
(wt%)

Average
grain size

1. Coarse-grained Ni (Ni 200)

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

nanocrystalline samples showed limited ductility with


measured elongation to fracture not exceeding about 8 %.
The same trends in the tensile properties were found at
the strain rate of 10-1/s. Significant strength enhancements
were attained, whereas the total elongation or ductility was
limited for the nanocrystalline samples in comparison with
the coarse-grained Ni (Fig. 2b). These observations of high
strength and reduced ductility are in agreement with
numerous previous experimental studies summarized in
previous review papers (e.g., [2, 28]). While the HallPetch
relationship accounts for the strengthening, low tensile
ductility is generally attributed to the lack of strain hardening required to resist macroscopic strain localization and
extend uniform plastic flow for nanocrystalline materials
(e.g., [9, 11]).
Table 2 summarizes tensile property values of all samples at the two strain rates, 10-2 and 10-1/s. For the coarsegrained Ni (32 lm), strain rate sensitivity is insignificant;
the key tensile properties, yield strength, ultimate tensile
strength and elongation remain virtually unchanged. When
varying the strain rate from 10-2 to 10-1/s, the nanocrystalline Ni (23 nm) showed YS increase from 950 to
970 MPa but essentially no change in UTS, indicating
some minor strain rate sensitivity. In comparison, the two
NiFe samples with smaller grain size of 16 nm displayed
evident sensitivity to the strain rate, showing an increase in
both YS and UTS at the higher strain rate.
Although a detailed analysis of strain rate sensitivity
was not the major focus of the current study, it should be
pointed out that the observed grain size dependent strain
rate sensitivity is in general agreement with previous
studies on nickel-based alloys (e.g., [28]). In a recent study
[29], the strain rate sensitivity, m, was examined over a
wide grain size range from 10 nm to 100 lm for Ni and
Ni-based alloys based upon extensive results from various

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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Table 2 Tensile properties at strain rate of 10-2 and 10-1/s


Samples

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)

studies with different testing methods, e.g., tensile tests at


different stain rates, stress relaxation [30] and strain rate
jump tests [31]. It was observed that the m values increased
significantly and ranged from 0.011 to 0.033 for materials
with average grain sizes between 10 and 50 nm, while in
the broad 50 nm100 lm range, the m value showed limited variation and remained below 0.005 [29] and within
the reported 0.0010.004 range for coarse-grained Ni [10].
This explains the insensitivity toward the strain rate for the
coarse-grained Ni (32 lm), and gradually increased
dependence on the strain rate for the 23 nm Ni and the two
16 nm NiFe alloys (Table 2).
The significant m value increase at very small grain
sizes for Ni-based materials can be attributed to deformation mechanisms other than the well-established dislocation-mediated (DM) mechanisms for coarse-grained
materials, owing to the close association between strain
rate sensitivity and underlying deformation mechanisms
(e.g., [3236]). Numerous experimental and simulation
studies have provided convincing evidence that dislocation
activity is negligible and deformation is dominated by
grain-boundary-controlled (GBC) mechanisms, such as
grain boundary sliding or grain rotation for nanocrystalline
materials with average grain sizes less than 10 nm (e.g.,
[28, 37, 38]). Therefore, it is plausible that in the current
study, DM mechanisms dominated in the deformation of
the coarse-grained Ni, whereas the 23-nm Ni and the two
16-nm NiFe samples deformed through both DM and
GBC mechanisms.
Strain localization
For conventional metallic materials, plastic deformation
during uni-axial tensile testing is normally expected to be
distributed uniformly at applied stresses lower than the
UTS; macroscopic localized deformation, necking, occurs
at the stress beyond the UTS [39]. In reality, the amount of
plastic deformation can vary from one location to another
well before the onset of necking. Digital image correlation
(DIC) strain measurement [40] has been shown to be an

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UTS
(MPa)

effective approach to examine in situ strain localization of


materials, i.e., it is capable of capturing the evolution of
localized strain during tensile testing. For example in an
earlier study, rapid evolution of shear banding was captured using the DIC approach for fully dense electrodeposited nanocrystalline Ni (grain size: 20 nm) during an
in situ tensile testing at quasi-static strain rate of 10-4/s
[41].
Figure 3 shows the results of DIC measurements at
different stages of deformation represented by five global
strains for the coarse-grained polycrystalline Ni of 32 lm
during tensile testing at a strain rate of 10-1/s. In the
contour map (Fig. 3a), the levels of local strain from low to
high are indicated by colors in a sequence of purple, blue,
green, yellow and red and the local strain field contours of
the coarse-grained Ni are mapped along the gauge section
at selected global strains indicated at the bottom of Fig. 3a,
up to the fracture strain of just over 50 %. Although uniform deformation is expected for the sample within the
global strain up to UTS at 45 % (Table 2), noticeable
variations of strain are displayed within the gauge length
even at low global strain of 15 % as indicated by two
colors, purple and blue.
As the global strain increases, the colors in the gauge
section keep changing due to intensified localized deformation. At the global strain of 35 %, still well within the
range of uniform deformation, the gauge section already
shows a range of different contour colors, indicating significant levels of localized strain. The highest level of
localization occurred during necking when imposed
deformation was concentrated essentially only in the
necking region. This is demonstrated in the contour map at
the fracture strain of 50 %, whereby the red area corresponds to the region of necking with very high local strain,
leading to fracture at the end of the tensile test (Fig. 3a).
Corresponding strain distributions along the gauge
length at the same global strains, i.e., 15, 25, 35, 45 and
50 %, respectively, are shown in Fig. 3b to present more
detailed information on the evolution of strain localization.
Note that the global strains do not always match with local

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(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

strain. Region 2 is approximately located between the two red-dotted


lines (Color figure online)

strain values, especially at low stress/strain levels. This


difference is somehow expected because of different
methods used in the strain measurements; global strain was
obtained indirectly from the crosshead displacement of the
tensile machine frame, while local strain values were
measured directly in the sample gauge section through the
DIC technique. It has been shown that strain values based
on crosshead displacement include contributions from
other sources, e.g., machine compliance and materials
outside the gauge length (e.g., those close to grip sections),
in addition to the strain of the sample gauge length [42]. As
a result, the measured strain based on the crosshead displacement almost always exceeds the actual strain in the
sample gauge section [42]. However, a discussion of
crosshead strain vs DIC strain is beyond the scope of this
study. The focus here is instead on the strain localization
within the stage of macroscopic uniform elongation, i.e.,
up to the global strain at UTS, a characteristic deformation
feature that can be reliably identified using crosshead

displacement. Hence, the disparity between global and


local strain has little impact in addressing strain localization for the samples in the current study.
Examination of the strain distribution curves reveals that
there are two deformation regions within the gauge section:
the region at the two ends, Region 1 and the region in the
center, Region 2. Due to its proximity to the grip section,
Region 1 is strongly influenced by its geometric confinement and has to accommodate the transition from close to 0
strain at the grip section to the imposed strain on the
sample. In other words, two factors contribute to the local
strain in Region 1, geometric conformation and material
properties. It appears that the geometric contribution
dominates the local strain in Region 1 as demonstrated by
the largely linear relationship between gauge location and
local strain with a slope increasing with the respective
imposed strain or global strain (Fig. 3b). This linear relationship of Region 1 ends where the strain transition to the
imposed value is accomplished; the end locations depend

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J Mater Sci (2014) 49:38473859

(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)

on the global strain and manifest themselves in the area


with evident slope change. For example at the UTS global
strain of 45 %, the locations are approximately at the gauge
locations of 10 and 33 mm, respectively, as shown in
Fig. 3b. Region 2 is located between these two points,
where the geometric contributions diminish and local
strains result entirely from the material properties. Hence,
the analysis of strain localization evolution should focus on
the strain distributions in Region 2, identified approximately between the two dotted lines in Fig. 3b.
For the coarse-grained Ni, strain distribution appears
fairly uniform in most locations of Region 2 at the global
strain of 15 %. Slightly different local strain was displayed
between the gauge locations of 26 and 32 mm (Fig. 3b).
This strain disparity became more visible in the same
location at the global strain of 25 %, and gradually evolved
into a broader valley, with a local strain significantly different from the rest in Region 2 at 35 % global strain, even
though the sample was still well within the strain range of

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macroscopic uniform deformation (\45 %). When the


applied stress was above UTS, necking took place and
subsequent deformation concentrated in this area as demonstrated in the local strain distribution at the global strain
of 50 % (Fig. 3b). Immediately thereafter, fracture occurred at the location with peak strain of about 80 %, substantially higher than the global fracture strain just over
50 % (Fig. 3a, b).
A similar development of localized strain is observed in
the nanocrystalline Ni sample with 23 nm grain size. As
shown in the strain field contour maps of Fig. 4a, deformation appears to be fairly uniform across the gauge length in
the early stage up to a global strain of 2.5 %. The sample
exhibited notable differences in local strains at a global strain
of 3.5 % as indicated by two colors, dark and light blue. The
local strain became more pronounced at the UTS strain of
5.5 % (Fig. 4a). Upon necking, imposed deformation was
concentrated in the center, and at about 8.0 % global strain,
fracture occurred in the necking region (red area) at an angle

J Mater Sci (2014) 49:38473859

of 62 (dashed line) as shown in Fig. 4a. In comparison with


the coarse-grained Ni, necking on the nanocrystalline Ni
sample is less pronounced. Details on strain localization
evolution can be more clearly demonstrated from strain
distributions along the gauge length at given global strains.
Figure 4b shows the distributions at five global engineering
strain levels of 2.5, 3.5, 4.5, 5.5 and 7.5 % for the nanocrystalline Ni sample tested at a strain rate of 10-1/s.
Similar to the deformation of coarse-grained Ni, the
strain distribution in Fig. 4b can be divided into two regions
for the nanocrystalline Ni: Region 1 at the ends of the gauge
length with strong influence from sample geometric confinement and Region 2 (identified approximately between
the two red-dotted lines) representing intrinsic material
properties. It can be seen that the nanocrystalline Ni already
exhibited slight local strain variation somewhere between
the gauge length of 17 and 25 mm in Region 2 even at the
global strain as low as 2.5 %. As the global strain increased
from 3.5 to 5.5 %, i.e., still within the strain range of
macroscopic uniform deformation, the strain disparity
became more and more pronounced between this area and
the rest in Region 2. In the final deformation stage of
instability, the imposed deformation concentrated in this
area in the form of necking with the peak local strain
reaching about 14 % at the global strain of 7.5 %. At the
slightly higher global strain of 8.0 %, the sample fractured
at the location with the peak local strain (Table 2; Fig. 4b).
For the two 16 nm NiFe electrodeposits and all materials tested at a strain rate of 10-2/s, strain localization was
observed in a similar manner. Generally, all samples
showed not much difference in the development of strain
localization during tensile testing at both strain rates.
Despite the wide grain size range (16 nm to 32 lm) and
very different tensile strengths and measured elongation to
fracture values, strain localization invariably started during
the stage of macroscopic uniform deformation, much
earlier than the occurrence of the macroscopic strain
localization in all of them. Subsequent necking took place
close to the region where the strain localization initiated.
There is a good agreement on the strain localization
behavior observed here for the nanocrystalline samples and
a recent DIC investigation, also on electrodeposited
nanocrystalline Ni [41]. During tensile testing of a 20 nm
Ni, initiation of shear localization was observed during the
uniform deformation stage. Rapid shear-banding evolution occurred immediately after necking, the macroscopic
strain localization and was concentrated in the middle of
the gauge area, leading ultimately to sample fracture [41].
Stress-induced heat generation
When metals are plastically deformed, part of the plastic
work is dissipated as heat during the deformation process

3853

(e.g., [43, 44]). In the current study, temperature change


due to heat release was measured and recorded by the IR
detector at different global strain levels. Figure 5a shows
selected infrared images of coarse-grained Ni at various
global strain levels, indicated at the bottom in Fig. 5a of
the individual snapshots at a strain rate of 10-1/s.
With the increase of global engineering strain from 15 to
45 %, the localized temperature along the sample gauge
increased continuously as indicated by the color changes
from light blue to yellow and orange. Temperatures are
distributed in a relatively symmetrical fashion along the
gauge with the maximum located in the central region; the
dashed line at a global strain of 50 % indicates the position
of fracture, which coincides with the area of the highest
temperature (i.e., red color) and/or most heat dissipation.
Figure 5b shows the relationship between global strain
and the instantaneous increase in the maximum temperature, DTmax, on the gauge section during tensile testing at
the strain rate of 10-1/s. During the stage of macroscopic
uniform deformation, DTmax reached approximately
42 C at the UTS strain of 45 % (eu in Fig. 5b, i.e., the
onset strain of necking). For the initial range of deformation (045 %), the average rate of temperature increase was
low, \1 C for each percent of global strain. Subsequent
deformation resulted in a rapid local temperature increase
in the necking region up to 70 C for the DTmax at fracture
strain of 51 %. With the addition of the room temperature
of 25 C, the recorded maximum temperature in the gauge
length, Tmax, was approximately 95 C for coarse-grained
Ni at the end of room temperature tensile testing.
The measurements for the 23 nm grain size nanocrystalline Ni during tensile testing at the strain rate of 10-1/s
are summarized in Fig. 6. At global strains below 3.5 %,
there was a very limited amount of heat generation as
indicated by little color change in the corresponding
infrared images (Fig. 6a). The nanocrystalline Ni displayed
a discernible temperature increase starting at a global
engineering strain of 4.5 %. In the final stage of deformation, a narrow region of high temperature formed around
the fracture location (the dashed line at an angle of 62
along the loading axis), indicating a highly concentrated
hot spot for the nanocrystalline Ni. This is somewhat different from the coarse-grained Ni, for which a much
broader and more or less uniform temperature distribution
was observed in the deformation stage close to fracture
(Fig. 5a).
Regarding the evolution of the DTmax, the nanocrystalline Ni exhibited a qualitatively similar profile as the
coarse-grained Ni. As shown in Fig. 6b, the temperature
increase was low during the uniform deformation stage.
A steep climb in temperature initiated at the onset of
necking, 5.5 % global strain (eu), and all the way to the
point of fracture (8 %). Specifically, the net increase in

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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)

J Mater Sci (2014) 49:38473859


600

(a)

550

500

450

400

350

300

250

200

80

500

(b)
400

u
300
40
200

0
Tmax , C

Eng. stress, MPa

60

20
100

0
0

10

20

30

40

50

60

Global strain/Elongation, %

temperature was approximately 12 C during the first stage


of deformation from 0 to 5.5 % global strain, while a
maximum DTmax of 58 C was recorded at the strain very
close to the fracture strain of 8.0 % (Fig. 6b). With the
addition of 25 C for room temperature, the recorded
maximum temperature, Tmax, was therefore 83 C for the
nanocrystalline Ni during tensile testing.
The two NiFe samples generally exhibited heat generation behavior similar to the nanocrystalline Ni; the initial temperature increase before necking was low, and a
rapid increase was observed after necking up to fracture. In
addition, the generated heat was concentrated in the narrow
area of the gauge center, surrounding the ultimate fracture
line for the two nanocrystalline NiFe samples.
Table 3 summarizes the maximum recorded temperatures, Tmax, along with the global elongation recorded at
both strain rates for all materials. It is evident that all
samples experienced local temperature increases during
tensile testing, showing Tmax values noticeably higher than
the ambient testing temperature. Furthermore for a given
sample, the attained maximum temperature, Tmax, is

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reduced at lower tensile strain rate. This apparent effect of


strain rate on Tmax reveals the critical influence of heat
conduction on the process of strain-induced heat
generation.
As shown in Table 2, the yield strength, tensile strength
and elongation to fracture of the coarse-grained polycrystalline Ni remained virtually the same at the two strain
rates employed, namely 10-2 and 10-1/s. For the material
under scrutiny, same amount of strain-induced heat should
be generated during tensile testing at the both strain rates
due to identical sample size. Because of strain localization,
heat generation was generally not uniform and varied from
one location to another, resulting in heat flow from higher
to lower temperature regions. During tensile testing, the
sample grip sections experienced little deformation and
thus functioned mainly as heat sinks for any strain-induced
heat. In the final stage of necking, most of the heat was
generated in the necking region, i.e., the gauge center, and
was then conducted toward the grip sections at both ends of
the samples. Due to the finite heat conduction of Ni, temperature distribution became a strong function of testing

J Mater Sci (2014) 49:38473859

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Fig. 6 Temperature change in


the 23-nm nanocrystalline Ni,
a infrared images with the
dashed line at 8 % strain
indicating fracture location, and
b engineering stressstrain
curve versus the maximum
temperature increase 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)

600

550

500

450

400

350

300

250

200

70

1600

(b)
1200

50
40

800

30

0
Tmax , C

Eng. stress, MPa

60

20

400

10
0

0
0

Global strain/Elongation, %

Table 3 Localized strain and maximum temperature recorded during


tensile testing
Samples

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

Global strain (%)

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

Likewise, the different Tmax values observed at the two


strain rates for the 23 nm Ni and the two 16 nm NiFe
samples can be mainly attributed to the heat conduction. In
addition, temperature distribution/gradients in the nanocrystalline materials (Fig. 6a) are more concentrated/steeper than those in the coarse-grained counterpart (Fig. 5a).
This likely resulted from the facts that for the nanocrystalline electrodeposits, the duration of tensile testing was
shorter due to their reduced ductility, and the thermal
conductivity is lower, e.g., up to 25 % reduction as
observed in our recent study for a series of nanocrystalline
Ni with average grain sizes of 2550 nm [45].
Implication of the measured heat generation

duration, and thus, the recorded maximum temperature


depended on strain rate. Higher strain rate is equivalent to
shorter test duration and therefore more concentrated
in situ temperature distribution, leading to higher maximum temperature for a given material with the same input
of mechanical energy. Hence, the coarse-grained Ni
exhibited higher Tmax at the higher strain rate (Table 3).

Returning to the main focus of this study, the measured


Tmax values observed as a result of strain-induced heat
generation do not support thermal activation as an underlying mechanism for the grain growth during room temperature tensile testing reported in previous studies (e.g.,
[10, 18]). For instance, the highest temperature recorded in
the 23 nm grain size nanocrystalline Ni was approximately
83 C during tensile testing, well below 120 C, the

123

3856

J Mater Sci (2014) 49:38473859

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

where j and A are, respectively, thermal conductivity and


cross-sectional area; DQ/Dt is the heat flux, leading to the
temperature gradient, DT/Dx, along the heat conduction
path. The heat flux is associated with the rate of
temperature change, b = DT/Dt, through heat capacity Cp
at constant pressure,
DQ
DT
Cp
Cp b
Dt
Dt

Then, DTRes in the area can be assessed as follow by


combining Eqs (1) and (2), replacing Cp with specific heat
cp through Cp = mcp = qALcp, and assuming a
symmetrical areal temperature distribution (Dx = L/2)
and negligible ambient heat exchange,
DTRes

qcp L2
b
2j

where L and q are the feature length of the resolution area


(50 lm) and material density, respectively. Some of the
parameters, e.g., cp and b, can have a range of values. In such
cases, the values are chosen to maximize DTRes for the
nanocrystalline Ni. Here, the upper value of cp = 0.56 J/g K
is used, based on the reported cp value range of
0.460.56 J/g K within 25200 C for nanocrystalline Ni
[46]. The handbook value of q = 8.89 g/cm3 for coarse-

123

grained Ni [47] can be used here because the density of fully


dense nanocrystalline Ni is grain size independent [48]. The
reported value of j is 90 W/m K for coarse-grained Ni [49].
Grain size reduction to about 25 nm resulted in 25 %
reduction of j or j = 67.5 W/m K for the nanocrystalline
Ni-based on recent observations [45]. The value of b can be
obtained from the slope in the plot of temperature vs strain.
For example in Fig. 6b, the largest slope section is located
at the top or the final stage of deformation, corresponding to
a rate of 635 K/s. Consequently, these values can be used to
calculate an upper bound value of DTRes of approximately
0.1 C. This is insignificant with respect to the measured
Tmax of 83 C for the nanocrystalline Ni. In other words, the
uncertainty due to the spatial resolution of the infrared
camera is expected to be insignificant in the Tmax measurements in the current study.
Another critical parameter is the time or duration available for thermally activated grain growth. In Ref. [10], the
observed growth from 20 to 200 nm grain size during room
temperature tensile testing at a strain rate of 103/s on the
nanocrystalline Ni occurred over a duration shorter than
10-4 s, corresponding to a rapid growth rate of more than
106 nm/s. This is in contrast to the actual growth rate
observed in an in situ TEM study on electrodeposited Ni
(as-deposited grain size: 20 nm) isothermally annealed at a
much higher temperature, 420 C [50]. In this study, it was
shown that grain boundary (GB) migration occurred as a
series of discontinuous steps followed by periods of
boundary stagnation; the GB velocity profile was represented by a series of delta functions. With a video sampling
rate of 30 frames per second, the highest recorded instantaneous GB migration rate was 700 nm/s, while most grain
boundaries migrated at a rate below 300 nm/s for the
nanocrystalline Ni at 420 C [50]. Much lower average
growth rates were observed in an ex-situ TEM study on a
series of nanocrystalline Ni-based electrodeposits, whereby
the same Ni sample as in Ref. [45] showed the fastest
average growth rate of only 33 nm/s after 5 s of isothermal
annealing at 420 C [51]. Note that the nanocrystalline Ni
samples used in Refs. [10, 50, 51] were all produced by the
same Integran electrodeposition process and exhibited the
same as-deposited average grain size (20 nm), similar grain
size distributions and likely similar impurity (e.g., S and C)
contents. Therefore, not much difference is expected in the
thermal behavior and stability for the Ni samples of the
three studies. Yet huge differences in growth rates, at least 3
orders of magnitude (106 vs. 700 nm/s), were observed
among the three studies. This indicates a different activation
mechanism for the grain growth shown in Ref. [10] than the
thermally activated growth observed in Refs. [50, 51].
Overall, the measurements of Tmax in the current study
and the growth kinetics comparison between previous
studies on very similar materials suggest that thermally

J Mater Sci (2014) 49:38473859

activated grain growth during room temperature tensile


testing for nanocrystalline nickel is highly unlikely. Hence,
the reported grain growth during tensile testing in previous
studies may be attributed to other contributing processes,
e.g., stress-induced grain growth.
In early studies on superplastic deformation, stressinduced grain growth was reported in conventional coarsegrained materials (e.g., [52, 53]). Given the significance of
grain size in nanostructures, this type of grain growth has
been an on-going focus of numerous experimental and
molecular dynamics simulation (MD) studies on nanocrystalline materials in recent years, [5466]. Evidence has
been presented for stress-induced grain growth through
direct experimental observations. For instance, stressinduced grain rotation and growth were observed during
in situ TEM tensile testing on nanocrystalline Ni electrodeposits [54, 63]. Again, the materials used in Ref. [63]
were produced by the same Integran electrodeposition
process as the one in the current study. In another in situ
TEM study, grain growth occurred upon nanoindentation in
nanocrystalline Al films [57]. Additionally, grains were
found to grow faster at cryogenic temperature than at room
temperature in a study on strained nanocrystalline Cu [58].
Further, it was recently concluded, based on the results of
tensile testing coupled with transmission electron microscopy on nanocrystalline Al films that grain growth was a
shear stress-driven process [64]. Generally, the experimental observations were in agreement with the results
from MD studies, e.g., on nanocrystalline Pd [54], Cu [56]
and Ni [62, 66].

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

As per DIC measurements, the samples with grain sizes


ranging from 16 nm to 32 lm exhibited similar strain
localization behavior. Local strain variations initiated in
the early stages of macroscopic uniform deformation
and became more pronounced close to the point of peak
load or UTS. Subsequent necking took place in the region
where significant strain localization initiated. Material
grain size showed little influence on strain localization
behavior. Some grain size dependent strain rate sensitivity
was observed during the tensile testing at two strain rates of
10-1 and 10-2/s. While the coarse-grained Ni exhibited
insensitivity to strain rate, gradually increased strain rate
sensitivity was demonstrated in the 23 nm grain size Ni
and the two 16 nm grain size NiFe samples. This sensitivity suggests that both dislocation-mediated and grainboundary-controlled mechanisms were operative in the
deformation of the nanocrystalline Ni and NiFe samples.
Acknowledgements The authors would like to thank Dr. David
Backman, Mr. Richard Bos and Mr. Thomas Sears from the National
Research Council, Institute of Aerospace Research for their help and
many valuable suggestions during the DIC and infrared experiments.
YZ would like to thank Mr. Cho for the fruitful discussion on thermal
and electric transport in nanocrystalline metals. Highly appreciated is
the financial support by the Natural Sciences and Engineering
Research Council of Canada (NSERC) and the Ontario Research
Fund (ORF).

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