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To cite this article: Li-Na Zhu, Bin-Shi Xu, Hai-Dou Wang & Cheng-Biao Wang (2015)
Measurement of Residual Stresses Using Nanoindentation Method, Critical Reviews in Solid State
and Materials Sciences, 40:2, 77-89, DOI: 10.1080/10408436.2014.940442
Table of Contents
1. INTRODUCTION........................................................................................................................................... 2
*E-mail: wanghaidou@aliyun.com
Color versions of one or more of the figures in this article can be found online at www.tandfonline.com/bsms.
77
78 L.-N. ZHU ET AL.
6. CONCLUSIONS ............................................................................................................................................11
FUNDING.............................................................................................................................................................11
REFERENCES......................................................................................................................................................11
1 1 ¡ n2 1 ¡ n2i
D C ; (3)
Er E Ei
where E and Ei are the elastic modulus of the specimen and the
indenter, respectively and v and vi are the Poisson’s ratio of the
specimen and the indenter, respectively.
A crucial step in calculating the hardness and elastic modu-
lus is the determination of the contact stiffness at the initial
unloading and the projected contact area at the peak load. The
unloading curve is usually well approximated by the power
law relation:
P D aðh ¡ hr Þm ; (4)
X
8
Ac D Cn ðhc Þ2 ¡ n D C0 h2c C C1 hc C L C C8 h1=128
c ; (8)
nD0
kP3max
HWt D (9)
9Wt2
kP3max
H Wp D ; (10)
9Wp2
4. NANOINDENTATION MODELS FOR THE This model is based on the difference of contact area
DETERMINATION OF RESIDUAL STRESS between a stress-free material and the same material with
At present, there is no one set method that can be applied to residual stress. When indented to the same depth, the contact
the calculation of residual stress for all materials. In this sec- area of material with compressive stress is larger than that of
tion, six typical models usually used to quantitatively deter- stress-free material, while smaller for tensile stress.
mine residual stress from analyzing load-depth curves are Note that there is a coefficient difference (sina) between the
discussed, including Suresh model, Lee models, Xu model, calculation formulae for tensile stress and compressive stress.
and Swadener models. Because the effects of tensile stress and compressive stress on
the indentation process are different, as shown in Figures 8
4.1. Suresh Model and 9. It is obvious that sA is the difference of load in the z
The residual stresses (tensile or compressive) are assumed direction between the materials with and without tensile stress,
to be equibiaxial and the magnitude is uniform over a depth while sAsina is the difference of load in the z direction
which is at least several times larger than the indentation con- between the materials with and without compressive stress.
tact diameter. The prerequisite of the model is that the material Before calculating the magnitude of residual stress using the
hardness H is unaffected by any pre-existing residual stresses. Suresh model, the residual stress state (tensile or compressive)
The relation between the residual stress s and the ratio of the should be determined from the loading curves for the stressed
real contact area A of material with residual stress to that of and stress-free specimens. Figure 10 shows the loading curves
stress-free material A0 can be written as for the stressed and stress-free 1045 steels at a fixed depth of
230 nm. It is concluded that the residual stress in the stressed
steel is compressive, because the material with compressive
A0
sDH ¡ 1 for tensile stress (14) residual stress requires larger force to be indented to the same
A
depth as the one without residual stress.65 According to Eq.
H A0 (15), the residual stress in the stressed steel was ¡117 § 20
sD 1¡ for compressive stress: (15)
sin a A MPa, which was in good agreement with that by the traditional
4.2. Lee Models model II when the stress ratio k D 1, namely, equibiaxial stress
4.2.1. Lee Model I state.
In 2003, Lee et al. proposed a new model based on stress
relaxation theory to determine equibiaxial residual stresses. 4.2.3. Application of Lee Models
Keeping the penetration depth constant, relax the residual The nanoindentation tests were performed on the cross-sec-
stress from the initial value s r to zero. tions of stressed and unstressed thermal barrier coating (TBC)
The residual stress can be calculated from the stress- samples.72 The unstressed sample was obtained by immersing
induced normal load and load difference between the materials the stressed sample in hydrochloric acid to dissolve the 304
with and without residual stress: stainless steel substrate. The residual stress in the TBC was
compressive since the coefficient of thermal expansion of the
ðP0 ¡ P1 Þ2
sr D 3
2 R3 P41 C ðR2 ¡ R3 P0 ÞP31 C ðR1 ¡ R2 P0 ÞP21 C ðR0 ¡ R1 P0 ÞP1 ¡ R0 P0 ; (16) TBC is less than that of metal substrate. As the indentations
were performed on the cross-section of the TBC, the compres-
sive stress applied on the indenter can be considered as a uni-
where P0 and P1 are the peak loads for the stress-free material
axial stress. Thus, the residual stress in the TBC was
and the material with residual stress. R0, R1, R2, and R3 are fit-
calculated using Eq. (17), k D 0. The results showed that the
ting constants between the contact area and peak load.
compressive stresses in the top coat (TBC) decrease from the
bonding coat (BC)/TBC interface to the top surface of TBC. It
4.2.2. Lee Model II
is obvious that the Lee model can evaluate the distribution of
In 2004, Lee et al. proposed another model to calculate the residual stress in micro scales.
non-equibiaxial surface stresses. Six different stresses were X. Zhao et al.57 investigated the residual stresses in TBCs
applied to the specimens using a special apparatus and divided by photoluminescence piezospectroscopy (PLPS) and nanoin-
into four categories (see Table 1): uniaxial stress dentation. The residual stresses obtained by nanoindentation
(s rx 6¼ 0; s ry D 0, 3# and 5#), equibiaxial stress (s rx D s ry 6¼ 0, 1# have similar trend with those calculated from PLPS measure-
and 6#), biaxial stress (s rx 6¼ s ry 6¼ 0, 2#), and pure shear stress ments. However, X. Zhao et al pointed out that the Lee model
(s rx D ¡ s ry 6¼ 0; 4#). s ry can be expressed as ks rx using a stress is only valid for a homogeneous material. As the TBC is far
ratio k, i.e. k D s ry =s rx , where k ranges from ¡1.0 to 1.0. from homogeneous, the residual stresses calculated by nanoin-
The biaxial stress can be separated into an equibiaxial stress dentation are only approximation.
and a pure shear stress. As the pure shear stress has no effect M.K. Khan et al.37 determined the residual stresses in
on the indentation load, the measurement of biaxial stress can Al-cladding and Al 2024-T351 by the Suresh and Lee models.
be simplified as an equibiaxial problem. The biaxial stress can The residual stresses from both of the Suresh and Lee models
be calculated as agree well with those from finite element simulation. The
divergence of the residual stresses on the far ends of the com-
3ð P0 ¡ P1 Þ pressive and tensile regions is due to that the Suresh model
s rx D ; (17)
ð1 C k ÞAc describes a nonlinear relationship and the Lee model considers
linearity in these regions.
where P0 and P1 are the peak loads for the stress-free material Like the Suresh model, the Lee models also require a stress-
and the material with residual stress. Ac is the contact area of free reference sample, although non-equi-biaxial surface stress
stressed material. Actually, Lee model I is the same as Lee can be determined. In addition, the models are based on a
stress-relaxation theory, i.e., the residual stresses are deter-
mined from the changes in applied load during stress relaxa-
TABLE 1
Unstressed reference and six different stressed states. tion at fixed indentation depth. However, the indentation
process is often considered as an elasto-plastic problem and
(Ó Elsevier. Reproduced with permission of Lee and Kwon.43
residual stress cannot be relaxed alone when keeping the depth
Permission to reuse must be obtained from the rightsholder)
invariable, because the stress-relaxation process can lead to a
Stress state s rx (MPa) s ry (MPa) k D s ry =s rx simultaneous change in the indentation load and depth.65
Reference 0 0 Unstressed
linear relationship with the ratio of residual stress to yield where R is the indenter radius; a the contact radius; s y the
stress, s r/s y, as shown in Figure. 11. In addition, the slope of yield stress. Obviously, if s y is available, the residual stress
the he/hmax vs. s r/s y depends only on the E/s y ratio. The fol- can be determined by Eq. (20) with experimental measurement
lowing equation can be used to relate the he/hmax ratio with the of (Era/s yR)0, which can be determined using least squares
s r/s y ratio: regression curve fits of hr/hmax D A1 C A2log(Era/s yR), as
shown in Figure 12.
he sr
D ¡ a C b; (18) 4.4.2. Swadener Model II
hmax sy
Swadener model II is based on the empirical Tabor relation-
where a and b are fitting constants, a is the slope of he/hmax vs. ship between hardness and yield stress,
s r/s y curves, and b is the intercept of he/hmax vs. s r/s y curves
at s r D 0. a depends only on the E/s y ratio, and the relation- H D Cs y ; (21)
ship between them follows a power law relationship:
¡ 1:25
E
a D 10:53 : (19)
sy
where C is the constrain factor. For stressed materials, Eq. 5. INDENTATION FRACTURE TECHNIQUE FOR THE
(21) should be rewritten as DETERMINATION OF RESIDUAL STRESS
When a brittle material is indented using a moderate force,
a permanent impression is often formed with radially oriented
cracks at the indent corner, as shown in Figure 13.74 Based on
H C s R D Cs y : (22) the classic indentation fracture mechanics, the fracture tough-
ness Kc of elastic-plastic brittle materials is directly related to
the indentation load P and the length of the radial cracks at the
By establishing the variation of Cs y with Era/s yR through surface, c0. For stress-free materials, the fracture toughness
experiments in a reference material in a known stress state, can be determined using the following expression:
then the residual stress can be calculated from measurements
of hardness.
P
Kc D x 3=2
; (23)
4.4.3. Limitation of Swadener Models c0
Swadener model I has an advantage that the measured
depth at which yielding occurs is affected by the stress in a
where x is the dimensionless residual stress factor which is
manner that can be analyzed by Hertzian contact mechanics.
related to the ratio of elastic modulus to hardness (E/H). It is
However, this model requires that the yield stress of materials
given by
be known in advance and that data be extrapolated outside the
range of experimental accessibility.73
Swadener model II can be used to measure residual
x D ξ 0 ðcotuÞ2=3 ðE=H Þ1=2 ; (24)
stresses in bulk materials to within 10–20%, but it cannot
be easily applied to thin films.73 The stress-free reference
specimen must be structurally identical to the tested speci-
where ξ 0 is a dimensionless constant, and u is the indenter
men if accurate residual stress measurements are to be
half-angle.
made. Unfortunately, this is often difficult to achieve in
For materials with preexisting residual stress s, the fracture
practice. For bulk materials, there is no substrate influen-
toughness is
ces. However, the substrate greatly affects the measure-
ment of thin film residual stresses. The substrate effects
can be alleviated when the indenter radius is on the order P
of or less than the film thickness. Kc D x § csc1=2 ; (25)
c3=2
Table 2 gives a comparison of the above six models. It is
obvious that the models can characterize only equibiaxial
stress or biaxial stress, while the stress along specimen depth where c is a dimensionless constant which can be obtained
cannot be obtained. Moreover, the six models all have limita- from the crack shape, and c is the crack length for the stressed
tions. Except Swadener model I, the other models requires a material. The first term on the right hand of Eq. (25) is the
reference specimen, which is often difficult to obtain. For stress intensity factor due to the indentation load, while the
Swadener model I, although a reference specimen is not second term is the stress intensity factor due to the residual
required, the yield stress must be determined by extra stress. Note that the second term is added to the first term for
experiment. tensile stress and subtracted for compressive stress.
TABLE 2
Comparison of six commonly used models to characterize residual stress
Indenter Characteristic Scope of
Models type parameters application Limitations
6. CONCLUSIONS
Residual stresses are increasingly desired to be measured
using a nanoindentation technique. There is no one set method
that appears to work for all materials. Six major models from
analyzing load-depth curves and indentation fracture tech-
nique have been developed. Unfortunately, the six models
involving Suresh model, Lee model I, Lee model II, Xu model,
Swadener model I, and Swadener model II all have limitations.
The Suresh model and Lee model I are restricted to equi-biax-
ial residual stress. Lee model II accounts for a general residual
stress state but cannot describe the well-known nonlinearity.
Xu model requires a special three-point bending device and
limits the application to very soft materials with high E/s y
ratios. Swadener model I requires that the yield stress of mate-
rials be known. Swadener model II cannot be applied to thin
films. The indentation fracture technique is destructive and
only applicable to brittle materials. Therefore, in order to eval-
uate residual stresses accurately, new methods should be
developed in the future. The methods with non-destructive and
FIG. 13. Typical indent with radially-oriented cracks. (Ó universal characteristic should be the research direction.
Elsevier. Reproduced with permission of Yen et al.74 Permis-
sion to reuse must be obtained from the rightsholder.)
FUNDING
For a given indentation load P, the residual stresses can be
determined by combining Eqs. (23) and (25): This article was financially supported by NSF of Beijing
(3120001), NSFC (51275105), and Distinguished Young
" # Scholars of NSFC (51125023).
1 ¡ ðc0 =cÞ3=2
s D Kc for tensile stress (26)
cc1=2
" #
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