Materials Science & Engineering A 751 (2019) 35–41

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Nanoindentation creep behavior and its relation to activation volume and T

strain rate sensitivity of nanocrystalline Cu
⁎ ⁎
Weiming Suna, Yue Jianga, Guixun Suna, Jiangjiang Hub, , Tianyi Zhouc, Zhonghao Jianga, ,
Jianshe Liana
a
Key Laboratory of Automobile Materials, College of Materials Science and Engineering, Jilin University, Nanling Campus, Changchun 130025, China
b
College of Mechanical Engineering, Zhejiang University of Technology, Hangzhou 310014, China
c
IMI Precision Engineering, Shanghai 201108, China

A R T I C LE I N FO A B S T R A C T

Keywords: The creep behavior of nanocrystalline Cu with an average grain size of 25 nm was investigated by na-
Nanocrystalline Cu noindentation test at room temperature. Using the creep strain rate versus creep stress data obtained at different
Nanoindentation creep behavior loading rates, the activation volume and strain rate sensitivity were determined obtained by cooperating the
Activation volume continuous stiffness measurement (CSM) technique. The results showed that the activation volume first increases
Strain rate sensitivity
and then decreases, and the strain rate sensitivity first decreases and then increases with increasing the creep
Grain boundary
stress. The experimental activation volume and strain rate sensitivity versus the creep stress data exhibit very
Dislocation
good agreements with the theoretical values calculated by the previous models, respectively. The analysis based
on the data of the activation volume and strain rate sensitivity revealed that at lower stress, the grain boundary
activities dominate and lead to the lower creep strain rates; at higher stress, the dislocation activities dominate
and lead to the higher creep strain rates. The analysis based on the data of the nanoindentation test also revealed
that the use of the CSM technique can lead to the continuous creep strain rate versus creep stress data, which
allows us to uncover the creep mechanisms over a wide range of the creep stress from the initial to steady stage.

1. Introduction thermally activated to move the dislocations over localized obstacles in

For coarse grained (CG) metals, plastic deformation is mediated by
nucleation and movement of intragranular dislocations. Interactions of
dislocations on intersecting slip planes create permanent dislocation
network that hinders further the movement of dislocations and thus
hardens materials. However, such dislocation activity is no longer
possible in nanocrystalline (NC) metals and is replaced by emission of
dislocations from grain boundary (GB) sources and their propagation
across the grains and eventual absorption in the opposite GBs [1–5]. On
the other hand, GB-mediated process such as GB sliding and GB diffu-
sion can take place concurrently with the dislocation activity [6–8].
Complicated interactions between the GB and dislocation mechan-
isms also result in difficulty in identifying which of them dominates in a
mechanical experiment with given experimental condition. The acti-
vation volume (V *) and strain rate sensitivity (m) are two important
parameters in the description of the kinetic and thermodynamic char-
acteristics of a plastic deformation process and have been widely used
to uncover the plastic deformation mechanisms of different metals and
alloys [9–13]. V * is the number of atoms that have to be coherently
their slip planes [14]. m is a sensitivity parameter of stress to strain rate
during plastic deformation and it can reflect a time or rate-dependent
deformation process [8]. V * and m can shed light on the thermally
activated transition of plastic deformation mechanism with strain rate
[15,16]. It is generally believed that a smaller V * and a larger m can be
expected when the GB deformation process is activated at lower strain
rates and, in contrast, a larger V * and a smaller m can be expected when
the dislocation activity dominates at higher strain rates. Therefore, the
change of V * and m suggests a transition in plastic deformation me-
chanism.
By using different testing methods, the stress dependences of the V *
and m values were obtained on different NC and ultrafine grained
(UFG) materials, e.g., compressive test on UFG Cu [17], strain-rate
jump test on UFG Cu [18], stress relaxation tests on NC Ni [19] and UFG
Ta [20], and nanoindentation creep tests on NC Ta [21], NC Ni [22],
UFG Ti [23] and CoCrFeCuNi high-entropy alloy [24]. It is noted from
these tests that the resultant V * and m values exhibit the either
monotonous increase or monotonous decrease except for the UFG Cu
[17] whose V * increases and then decreases with stress. Duhamel et al.

⁎
Corresponding authors.
E-mail addresses: jiangjiangwho@gmail.com (J. Hu), jzh@jlu.edu.cn (Z. Jiang).

https://doi.org/10.1016/j.msea.2019.02.027
Received 18 October 2018; Received in revised form 8 February 2019; Accepted 8 February 2019
Available online 10 February 2019
0921-5093/ © 2019 Elsevier B.V. All rights reserved.
W. Sun, et al.
[18] proposed a theoretical model to investigate the dependence of V *
on opening plastic deformation mechanisms. This model predicts that
when the plastic deformation of a material is mainly controlled by GB
activities, V * will be very small and increase with increasing the stress
and, in contrast, when the plastic deformation is mainly controlled by
dislocation activities, V * will decrease with increasing the stress. This
means that V * should be a continuous and non-monotonous function of
the stress. Similar dependence of m on the stress was also suggested by
Champion [17]. However, as mentioned above, few of the existing
experimental data of V * and m [17–24] showed such stress dependence
even GB and dislocation mechanisms are effectively activated. Possible
reasons for the lack of such dependence are the limitation in the testing
method and the insufficient range of the stress tested.
In this paper, the dependence of V * and m on creep stress of a na-
nocrystalline Cu with an average grain size of 25 nm was investigated
by nanoindentation creep test cooperating the CSM technique in a wide
range of loading rates at room temperature. The creep strain rate versus
creep stress data were obtained. Using these data, the two relationships
between the V * and m values and creep stress were determined. These
two relationships were compared with the theoretical models [17,18].
Based on the V * and m data, the creep mechanisms were analyzed.
Finally, some important features of the current nanoindentation testing
methods were discussed.
2. Experiments
The NC Cu used in this text was prepared by electric brush-plating
technique and the synthetic process was described in Ref. [9]. This NC
Cu consists of roughly equiaxed grains with random crystalline or-
ientations and predominant high-angle GBs. The purity and density of
the NC Cu are ~99.73 wt% and ~8.93 g/cm3, respectively. The main
impurities, in wt%, are 0.060C, 0.054O, 0.023H, 0.056N, 0.001S and
0.001P. Fig. 1(a) and (b) shows the TEM bright-field image of the NC Cu
and the grain size distributions, respectively. As shown, this NC Cu has
a narrow grain size distribution with an average grain size (d) of 25 nm.
Nanoindentation tests were performed on a nanoindenter (KLA-
Tencor Nanoindenter G200) with a Berkovich diamond indenter at
room temperature. The surface of NC Cu was mechanically polished to
mirror finishing to acquire reliable data. The area function of the in-
denter had been calibrated on the standard fused silicon before na-
noindentation tests. The contact stiffness (S ) as a function of indenter
displacement was obtained by the CSM technique, via loading strain
rates of 0.5, 0.05 and 0.005 s−1 and a maximum displacement of
2000 nm. Nanoindentation creep tests were performed at a wide range
of loading rates (P ̇ ) from 0.05 mN/s to 500 mN/s to a peak load of 300
mN with a holding time of 1000 s. The indenter was unloaded to 10% of
the maximum load and held for 500 s for thermal drift correction to
minimize its negative influence on the displacement measurement [25].
Fig. 1. The TEM bright-field image of the NC Cu (a) and the grain size distributions (b).
36
Materials Science & Engineering A 751 (2019) 35–41
The nanoindentation tests were repeated at least ten times under the
same conditions.
3. Results and discussion
3.1. Creep behavior
Fig. 2(a) shows the representative load versus displacement (P − h )
curves obtained at the P ̇ of 0.05 mN/s to 500 mN/s. In the loading
regime, h at given P increases sharply with decreasing P ̇ . In the holding
regime, the P − h curves exhibit wide load plateaus (large creep dis-
placement (hcreep )). Fig. 2(b) shows the corresponding creep displace-
ment versus holding time (hcreep − tH ) curves in the holding regime. The
h − t data in the holding regime can be well fitted by an empirical
equation
r
h = p + q ln ⎛ − 1⎞
⎝t − s ⎠ (1)
where p , q , r and s are the fitting parameters. The representative fitting
h − t curves and the experimental data in the holding regime at
P = 500 mN/s, 5 mN/s and 0.05 mN/s are shown in Fig. 2(c), (d)
and (e), respectively. It can be seen that the fitting curves show good
agreements with the experimental data. The creep strain rate (εḢ ) can
be expressed as [26]
1 ∂h
εḢ =
h ∂t (2)
Fig. 2(f) shows the creep strain rate versus holding time (εḢ − tH )
curves obtained from the h − t curves in the holding regime. It is seen
that εḢ drops rapidly with increasing tH , and then decreases slowly in
the subsequent steady-state creep regime. At given tH , εḢ increases with
increasing P ̇, which indicates that the creep behavior depends strongly
on P ̇ .
Fig. 3(a) and (b) show the representative load versus displacement
(P − h ) curves and the corresponding contact stiffness versus dis-
placement (S − h ) curves obtained by the CSM technique at the loading
strain rates of 0.5, 0.05 and 0.005 s−1, respectively. It can be seen that S
is independent of loading strain rate. Fig. 4 shows the creep stress
versus time (σH − tH ) curves in the holding regime obtained by using
the following equation [26,27]
P
σH =
3Ac (3)
where Ac is the contact area. Ac can be expressed as [26,27]
Ac = C0 hc2 + C1 hc + C2 hc1/2 + C3 hc1/4 (4)
where C0 , C1, C2 , C3 are the fitting parameters and hc is the contact
depth. In this work, the fitting parameters are C0 = 24.3, C1 = 5115.9,
C2 = 10088.2 and C3 = −38910.5 which were obtained by the area
W. Sun, et al. Materials Science & Engineering A 751 (2019) 35–41

Fig. 2. The load versus displacement (P − h ) curves (a) obtained at a maximum load of 300 mN and holding time of 1000 s at different P ̇ . The corresponding creep
displacement versus holding time (hcreep − tH ) curves (b), the experimental displacement versus time (h − t ) curve and the fitted curve obtained at Ṗ = 500 mN/s (c),
P ̇ = 5 mN/s (d) and P ̇ = 0.05 mN/s (e) and the creep strain rate versus holding time (εḢ − tH ) curves (f) in the holding regime.

function calibration procedure. hc can be expressed as [26,27] 3.2. Determinations of activation volume and strain rate sensitivity

εP
hc = h −
S (5)
where ε is a constant. For the Berkovich indenter in this work, ε = 0.75
[27]. In the calculations of σH (Eq. (3)), the S − h data obtained by CSM
technique in Fig. 3(b) were used to determine hc and Ac . As shown in
Fig. 4, σH decreases rapidly with increasing tH and then decreases stably
with increasing tH . σH has a larger dropping rate at higher P ̇ than that at
lower P ̇ , which indicates a more rapid stress relaxation at higher P ̇ than
that at lower P ̇ .
According to the results in Figs. 2(f) and 4, the εḢ and σH at the same
tH in the whole creep process can be obtained, so the εḢ versus σH data
were obtained at different P ̇ and the resultant εḢ − σH curves are shown
in Fig. 5(a). It is interestingly noted that the εḢ − σH data at different P ̇
mutually superimpose and εḢ increases with increasing σH . Based on
these εḢ − σH curves, the true activation volume V * can be expressed as
[28–30]
∂ ln εḢ ⎞
V * = MkT ⎛
⎝ ∂σ * ⎠ (6)

37
W. Sun, et al.
Fig. 3. The load versus displacement (P − h ) curves (a) and the corresponding contact stiffness versus displacement (S − h ) curves (b) obtained by CSM technology
at the loading strain rates of 0.5, 0.05 and 0.005 s−1.
Fig. 4. The creep stress versus holding time (σH − tH ) curves in the holding
regime.
where M is the Taylor factor, k is the Boltzmann constant, T is the
absolute temperature and σ* is the effective stress, which can be written
as σ * = σH − σi , where σi is the athermal long-range internal stress and
is usually approximated as a constant. So, Eq. (6) can be written as
∂ ln εḢ ⎞
V * ≈ MkT ⎛ ⎜ ⎟
⎝ ∂σH ⎠ (7)
By taking M = 3 [16,18,31], k = 1.38 × 10−23 J/K and T = 298 K
and using the εḢ versus σH data in Fig. 5(a), the variation of V * with σH
was obtained and the result is shown in Fig. 5(b). As shown, there are
two distinctive regions. In region I, V * increases with increasing σH
from 6b3 to a maximum value of 10.5b3 at 530 MPa, where b is the
Burgers vector of the dislocation and b = 0.256 nm for Cu [32]. In re-
gion II, V * decreases with increasing σH from the maximum value to
2.5b3 .
Using the εḢ versus σH data in Fig. 5(a), the variation of the strain
rate sensitivity m with σH , defined as [33,34]
∂ ln σH
m=
∂ ln εH˙ (8)
can be determined and the result is shown in Fig. 5(c). As shown, there
are also two distinctive regions. In region I, m decreases with increasing
σH from 1.04 to a minimum value of 0.8 at 530 MPa. In region II, m
increases with increasing σH from the minimum value to 1.2. It is noted
that the relationship between m and σH is contrary to the relationship
38
Materials Science & Engineering A 751 (2019) 35–41
between V * and σH .
3.3. Stress dependence of activation volume and strain rate sensitivity
Duhamel et al. [18] proposed a model in which V * is connected with
σ*. In this model, a critical stress σ0*, which can be expressed as
σ0* = Mβ Gb/ d , is proposed, where β is the material constant, G is the
shear modulus. When σ * ≤ σ0*, the plastic deformation is controlled
only by GB activities and the corresponding V * can be written as [18]
V * = VGB (9)
where VGB = 1b3 is the activation volume when the plastic deformation
is controlled only by GBs activities [28]. When σ * > σ0* , the plastic
deformation is dominated by both GB and dislocation activities and the
corresponding V * can be given by [18]
−1
σ * − σ0* δ C (σ0*)2 ⎞
V * = VGB + 2MkT ⎜⎛ + ⎟
⎝ B b σ * − σ0* ⎠ (10)
where δ = 2b is the thickness of GB, B and C are the fitting parameters.
The first and second terms in the bracket of the right of Eq. (10) re-
present respectively the contributions of the dislocation and GB activ-
ities to V *. B and C can be expressed as
δ ∂vGB
B=1+ >1
bd 2ve ∂ρ (11)
C=
νGB
Bνe (12)
where νe is the frequency of dislocation emission from GB, νGB is the
frequency of an elementary shear at GB companied with dislocation
absorption and ρ is the dislocation density. According to Duhamel et al.
[18], B and C can be approximately regarded as the constants, and C
can be determined by a condition in which the plastic deformation is
controlled only by GB activities. According to this condition, the term
(σ * − σ0*)/ B in Eq. (10) will be far smaller than the corresponding term
(δ C / b) σ0*2/(σ * − σ0*) and Eq. (10) can be written as
2MkTb
V * ≈ VGB + (σ * − σ0*)
δ C (σ0*)2 (13)
Eq. (13) indicates that C can be determined from the slope of the
experimental V * versus σH data when the relation of σ * − σ0* to σH is
determined. According to σ * = σH − σi and σi = σ0 − σ0* [18], one has
σ * − σ0* = σH − σ0 , where σ0 is the value of σH at which V * = 1b3 .
Therefore, σ0 can be determined by finding the crossover point of the
tangent of the V * versus σH curve in region I with the σH axis (see
Fig. 5(b)). From Fig. 5(b), σ0 is determined to be σ0 = 450 MPa. By
W. Sun, et al.
Fig. 5. Creep strain rate versus creep stress (εḢ − σH ) curves (a), activation
volume versus creep stress (V * − σH ) curves (b) and strain rate sensitivity
versus creep stress (m − σH ) curves (c) in the holding regime.
taking β = 0.5 and d = 25 nm, σ0* is calculated to be σ0* = 374 MPa .
Inserting σ * = σH − 76 MPa , σ0* = 374 MPa and the values of other
parameters into Eq. (13) and comparing with the slope value of the
experimental V * versus σH curve in region I (0.07b3 MPa−1), the C value
can be determined to be C = 0.02 .
Furthermore, inserting σ * = σH − 76 MPa , σ0* = 374 MPa , C = 0.02
and the values of other parameters, the V * versus σH curves were cal-
culated for different B values and compared with the experimental
curve. The comparison results in Fig. 6(a) show that the calculated V *
versus σH curves with B = 2.5 exhibits the best agreement with the
experimental curve.
39
Materials Science & Engineering A 751 (2019) 35–41
According to the relationship between the m and V *, i.e.,
m = MkT /(σH V *) [35], and the expressions for V * (Eqs. (9) and (10)),
the corresponding m can be written as [17]
MkT
m= (σH ≤ σ0)
σH VGB (14)
−1 −1
⎡σ V σ − σ0 δC σ02 ⎞ ⎤
m = ⎢ H GB + 2σH ⎛⎜ H + (σH σ0)
b σH − σ0 ⎠ ⎥
⎟
MkT ⎝ B (15)
⎣ ⎦
Inserting σ0 = 450 MPa and C = 0.02 and the values of other para-
meters, the m versus σH curves were calculated for different B values
and compared with the experimental curve. The comparison results in
Fig. 6(b) show that the calculated m versus σH curve with B = 2.5 ex-
hibits the best agreement with the experimental curve.
3.4. Explanations of activation volume and strain rate sensitivity
According to the work of Becker [35–37], V * can be written as
V * = b × ξ × l*, where ξ is the distance swept out by the mobile dis-
location during an activation event, which can be considered to be a
constant [35,38], and l* is the length of dislocation segment or the
distance between two pinning sites on GBs. Furthermore, as suggested
in Ref. [35], l* has two limits, i.e., when ρ is low, l* can be written as
l1* = χ d ; when ρ is high, l* can be expressed as l 2* = aρ−1/2 , where a and
χ are proportionality factors. There is the grain size across which me-
chanisms controlling plastic is different. This grain range is 10–500 nm.
This suggests that for the present NC Cu, the variation of l* depends on
the stress level and thus results in different dependence of V * on σH .
For NC metals, dislocation activities, including the nucleation from
GB sources, their propagation across the grains and eventual absorption
in the opposite GBs occurs when a critical stress is reached [1–5]. At
low stress, this critical stress cannot be satisfied, so the deformation
must be mediated by GB activities. In this case, l* is a very small con-
stant which are associated with the GB activities or some dislocation
activities within GBs or near GBs (see Fig. 7(a)), and a small V * value is
thus expected at low stress. As σH increases, GB dislocation sources
would be activated, and dislocations begin to nucleate from GBs and
propagate across the grains with their two ends depinning and shifting
along the GBs (see Fig. 7(b)). In this case, ρ is lower and l* is controlled
by l1* = χ d , where the χ value should be a stress dependent parameter
and 0 < χ ≤ 1. An increased l* or an increased V * would be expected
when σH varies in a range from 460 to 530 MPa. When σH reaches a
value larger than 530 MPa, would be effectively activated, the number
of the dislocations nucleated GBs increase significantly. An effective
dislocation storage inside the grain interior would occur due to the
enhanced nucleation of dislocations from GBs and the increased diffi-
culties for the dislocation absorption in the opposite GBs (see Fig. 7(c)).
In this case, ρ increases significantly and l* is controlled by l 2* = aρ−1/2 .
As a result, a decreased l* or a decreased V * would be expected when σH
is larger than 530 MPa. The above analysis clearly indicate that the
steady creep process at lower stress level is mediated mainly by the GB
activities, which is gradually replaced by the high speed creep process
mediated mainly by the dislocation activities.
According to the relation m = MkT /(σH V *) mentioned above, there
is an approximate relationship between m and 1/ V * since σH is not a
constant. Therefore, the variation in the m value with σH (Fig. 5(c)) and
its relation to the creep mechanisms can be similarly explained to those
for the V * value.
3.5. Some features of present nanoindentation creep tests
An important result of our nanoindentation creep test is that the
εḢ − σH curves obtained at different P ̇ mutually superimpose, which
allows us to obtain the continuous εḢ − σH data and hence the con-
tinuous V * and m versus σH data over a wide range of σH from 450 MPa
W. Sun, et al.
Fig. 6. Comparison of the activation volume versus creep stress (V * − σH ) curves obtained by experiment and Duhamel et al.’s model (a), and comparison of the
strain rate sensitivity versus creep stress (m − σH ) curves obtained by experiment and Champion's model with different B (b).
to 1350 MPa. It is noted that such V * and m versus σH data were less
reported. In the previous nanoindentation creep tests on NC and UFG
metals [21–24], the εḢ − σH curves obtained at different loading strain
rates or loading rates were discrete and did not mutually superimpose.
Although the m values obtained from the discrete εḢ − σH curves in
these studies are accurate as indicated by Eq. (7) and were used to
analyze the creep behavior in the steady stages, the range of σH covered
are narrow. The resultant V * and m values either increase or decrease
monotonously with increasing σH and the non-monotonous variation in
the V * and m value like that found in the present nanoindentation creep
test were less observed [17].
In general, for the creep deformation of a plastic material, there
should exist a certain relationship between εḢ and σH and the mutually
superimposed εḢ − σH curves should be thus expected. Because εḢ is
only related to the h − t data, the discrete εḢ − σH curves obtained in
the previous nanoindentation creep tests [21–24] indicate that the σH
data might be not measured accurately. In fact, for plastic materials,
especially NC and UFG metals, the creep deformation can occur not
only during the holding stage, but also in the unloading stage. A direct
consequence of the creep deformation in the unloading stage is that it
leads to a nose-shaped P − h curve in the initial unloading stage
especially when a slow unloading rate was used [39]. In this case, it is
difficult to obtain the accurate S data. An effective method for over-
coming this inaccuracy in the S data is to suppress the creep de-
formation by using the higher unloading rate as possible. Another so-
lution is to use CSM technique. It is believed that CSM technique can
obtain the accurate S − h data and such data is independent on the
unloading process [40,41]. Therefore, a possible reason for the discrete
εḢ − σH curves observed in the previous nanoindentation creep tests
[21–24] is the inaccurate σH data caused by the errors in the resultant S
Fig. 7. Schematic illustrations of the pinning-depinning mechanism of creep behavior.
40
Materials Science & Engineering A 751 (2019) 35–41
data. It is noted that in these tests [21–24], CSM technique was not used
and the unloading rates were not mentioned. In addition, it can be seen
from Fig. 3(b) that S increases linearly with h , while the S value
measured by the nanoindentation creep test is a single value. This is
also an important reason responsible for producing the discrete εḢ − σH
curves.
Because the continuous V * or m versus σH data can be obtained over
a very wide range of σH , the present nanoindentation creep test focuses
on the entire creep process and the variation in the relevant creep
mechanisms from the initial to steady stage can be more clearly un-
covered. This is obviously better than the previous nanoindentation
creep tests [21–24] in which only the creep process in the steady stages
were emphasized. In addition, it should be pointed out that the con-
tinuous strain rate versus stress data also can be similarly achieved in
the loading region when the load-controlling mode is used. Under this
mode, the strain rate varies with the loading stress. If such data can be
achieved, the corresponding activation volume or strain rate sensitivity
versus stress data can be obtained, which can be used to analyze the
variation of plastic deformation mechanisms during loading process,
which will be the future work of the present authors.
4. Conclusion
Nanoindentation tests were carried out to investigate the creep
behaviors of NC Cu with a grain size of 25 nm after deforming under a
wide range of loading rate at room temperature. Based on the re-
lationship between the creep strain rate and creep stress obtained at
different loading rates, the activation volume and strain rate sensitivity
versus creep stress data were determined by cooperating CSM tech-
nique. The results shows that the activation volume increases and then
W. Sun, et al.
decreases, and the strain rate sensitivity decreases and then increases
with the increasing creep stress. The experimental activation volume
and strain rate sensitivity versus the creep stress data are in good
agreements with the theoretical values calculated by the previous
models, respectively. The analysis based on the data of the activation
volume and strain rate sensitivity revealed that at lower stress, the grain
boundary activities dominate and lead to the lower creep strain rates, at
higher stress, the dislocation activities dominate and lead to the higher
creep strain rates. The analysis based on the data of the nanoindenta-
tion test also revealed that the use of the CSM technique can lead to the
continuous creep strain rate versus creep stress data, which allows us to
uncover the creep mechanisms over a wide range of the creep stress
from the initial to steady stage. Similar method of nanoindentation test
can be applied to the loading region.
Acknowledgments
This work was financially supported by the National Natural Science
Foundation of China (Grant Nos. 51371089 and 51271152).
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