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School of Mechanical and Aerospace Engineering, Oklahoma State University, Stillwater, OK, USA
Physikalisch-Technische Bundesanstalt, Braunschweig, Germany
Laboratory for Precision Machining (LFM), Bremen, Germany
A R T I C L E I N F O
A B S T R A C T
Keywords:
Surface
Nanoindentation
Mechanical property
Nanoindentation has emerged as an important method for the evaluation of the mechanical response of
small material volumes and thin lms to applied loading. Here, we present a review of the measurement
method, the instruments currently in use and the procedures for the analysis of the resulting data. The
methods developed for verication and calibration, including a discussion on uncertainty of parameters
are presented. The results of the most recent CIRP sponsored comparison on nanoindentation are
presented and compared to the results obtained in the rst such comparison. Examples of some of the
emerging uses of the technique are included.
2010 CIRP.
1. Introduction
* Corresponding author.
E-mail address: lucca@ceat.okstate.edu (D.A. Lucca).
0007-8506/$ see front matter 2010 CIRP.
doi:10.1016/j.cirp.2010.05.009
804
805
Fig. 3. Typical test force vs. test time cycle for indentation.
Fig. 4. Test force vs. indentation depth plot. See text for explanation of annotations.
test force the depth of the permanent deformation in the test piece
is given by hp, Fig. 5(b). The accurate determination of these depths
requires the accurate assessment of the zero point of the depth. The
ISO standard 14577 [33] species that the uncertainty in the zero
point determination should be less than 1% of the maximum
indentation depth for the macro and micro range. For the nano
range the uncertainty may be greater than 1%, however it should be
estimated and recorded.
The ISO standard further stipulates that the test piece should be
free of extraneous matter and should be aligned such that the
surface is perpendicular to the test force direction. The surface
should be prepared in such a way that alterations to the near
surface hardness are minimal. The surface roughness Ra of the test
piece should be less than 5% of the maximum indentation depth for
the macro and micro range. In the nano range this may not always
be possible. To exclude the inuence of the test piece support on
the measurement of hardness and elastic modulus the thickness of
the test piece should be greater than 10 times the maximum
indentation depth or 3 times the maximum indentation diameter,
whichever is greater.
2.2. Instruments
There have been a variety of instruments developed for
performing instrumented indentation; Table 1 shows a sample
of instruments that are currently commercially available. The
Fig. 5. Schematic drawing of indentation surface showing (a) indenter with applied
test force and (b) after removal of the test force. Indentation depth under applied
test force, h, depth of contact of the indenter with the test piece hc, depth below
surface not in contact with indenter hs and permanent indentation depth after
removal of test force hp, are denoted.
806
Table 1
Sample of indentation instruments and the measurement systems employed.
Instrument
Force measurement
system
Displacement
measurement
system
Electromagnetic
Electromagnetic
Electromagnetic
Capacitive
Capacitive
Inductive
Inductive
Inductive
Capacitive
Capacitive
Capacitive
Capacitive
Inductive
Inductive
Fig. 6. MEMS-based nanoindenter developed at the PTB [44]. (a) Schematic diagram
of the nanoindenter showing the electrostatic comb drive and (b) close-up of the
indenter holder where the indenter is a spherical ball of 100 mm diameter.
initial dislocation nucleation and subsequent dislocation multiplication. Fig. 7 shows frames from a video of the indentation
process where the indenter is at the bottom of the images and the
aluminum is above. The time from the start of the experiment is
shown in seconds in the upper right corner of the images. The rst
frame (a) shows that the aluminum is dislocation free in the area to
be indented. In (b) and (c), contact has been made however the
deformation is still elastic. Between frames (c) and (d), dislocations
are nucleated. In (e) and (f), the multiplication of dislocations is
shown. Indentation instruments have been modied to include
Table 2
The range and digital resolution of the force and displacement systems as given by
the manufacturers.
Instrument
Fmax (N)
Force
resolution
(nN)
hmax
(mm)
Displacement
resolution
(nm)
Picodentor HM500
Nano Indenter G300
Nano Test
Triboindenter TI 950
Ultra Nano Hardness Tester
IBIS Model B
UNAT
0.5
0.5
0.5
10a
0.1
0.05, 0.5
2
100
50
30
1
1
70
100
150
500
50
0.04
0.01
0.001
0.02
0.001
0.003
0.01
100
2, 20
150
Fig. 7. Still frames of video from TEM observation of indentation in aluminum [49].
Indenter is in the bottom portion of the frames and aluminum is above. Time in
seconds is shown in the upper right of each frame. Plastic deformation is initiated
sometime in between frames (c) and (d).
807
depth. The intercept of the depth axis by the tangent line to the
unloading curve determines the depth hr, as shown in Fig. 4. The
contact depth, hc, is calculated from:
hc hmax ehmax hr
(1)
F max
Ap hc
(2)
where Fmax is the maximum test force and Ap(hc) is the projected
area of contact of the indenter evaluated at a depth of hc. The
indentation modulus EIT can be calculated from the following two
equations:
EIT
Er
Fig. 8. Scratch test results for amorphous carbon lms (a-C:H) containing silicon.
The micrographs are for a 614 nm thick lm (top) and a 366 nm thick lm (bottom).
Large uctuations in the penetration depth are associated with spalling of the lm
[51].
1 ns 2
1=Er 1 ni 2 =Ei
p
p
p
2C Ap hc
(3)
(4)
g 1
1 2ns
41 ns tan f
(6)
808
Table 3
Properties derived from the instrumented indentation test.
Elastic or elasticplastic properties
Plastic properties
Fig. 9. Test force vs. indentation depth curve for the indentation of 1 0 1 0 ZnO
showing pop-in at a force of approx. 160 mN. After [62].
Fig. 10. Test force vs. indentation depth for indentations in (1 1 1)Si. The observed
pop-out and elbow in the unloading curve are attributed to phase
transformations of the silicon [63].
809
Fig. 13. Indentation hardness vs. normalized contact depth of DLC coatings on
hardened tool steel. The thicknesses of the coatings were ^ 2510 nm, &1470 nm
and ~ 460 nm [35].
Fig. 11. Indentation hardness vs. contact depth for two different surfaces of ZnO.
The hardness is found to exhibit the size effect, i.e., the hardness increases as the
indentation depth decreases. After [62].
Measurement methods
Indenter geometry
Test force
Indentation depth
Machine compliance
Indenter area function
Fig. 12. Plane strain indentation modulus vs. normalized contact radius of
Diamond-Like Carbon (DLC) coating on hardened tool steel [35].
Testing cycle
810
Fig. 15. Top view of silicon spring based device for the calibration of test force and
indentation depth [67].
Fig. 16. Nanoforce actuator with multifold springs [69]. Central shaft of actuator is
on the right of the image.
Table 5
Resolution and maximum permissible error of the displacement measuring system
[33].
Fig. 14. NIST electrostatic force balance: (a) complete system including vacuum
enclosure, (b and c) close-up of balance [66].
Range of
application
Resolution of the
displacement measuring
device (nm)
Maximum permissible
error
Macro
Micro
Nano
100
10
1
1% of h
1% of h
2 nm, preferably 1% of h
p 1
1
4 Er 2 C t C f 2
(9)
Ap hc C 0 hc C 1 hc C 2 hc
1=2
C 3 hc
1=4
C 8 hc
1=128
(10)
sq
q
(11)
Low
Medium
High
2500
25007000
>7000
50100
100450
811
Table 7
Maximum limits of the coefcient of variation for satisfactory repeatability of
indentation instruments [33].
Material
parameter
Micro range
0.2 mm h 1 mm
Macro
range
HM, HIT
EITa
5%
5%
2%
5%
2%
5%
For nearly perfectly plastic materials these limits may not be achievable.
(12)
r
s2 xk
(13)
812
N
X
@f 2
@xi
i1
u2 xi
(14)
1
Ap
u2 F max
HIT 2
Ap 2
u2 Ap
(15)
where Ap(hc) has been shortened to Ap for simplicity. Note that the
uncertainty terms u(Fmax) and u(Ap) should include all factors
which inuence the measured force and determination of the area
function. Hsu et al. performed this type of analysis for an
indentation instrument that operates in the nano range [76].
They found that the relative standard uncertainty of indentation
hardness was 6.3% and indentation modulus was 6.8% for
indentations with a depth of 100 nm or greater. In the micro
and macro range, Ullner analyzed the sources of uncertainty in the
instrumented indentation test for different materials [30,65]. The
material properties chosen corresponded roughly to those of iron,
aluminum, tungsten carbide and glass. Table 8 gives a summary of
the results obtained. The combined uncertainties for the macro
range were found to be less than those obtained for the micro
range. The Martens hardness determined from the slope of the
loading curve produced the highest relative uncertainty. Ullner
found that the machine compliance contributed signicantly to the
uncertainty in HMs [65]. He also found that the uncertainty in the
zero point determination could have a large inuence on the
combined uncertainty.
4. CIRP international comparison on nanoindentation
4.1. Introduction
By about 1990, nanoindentation was emerging as a useful
method for the determination of the micro or ultra-microhardness
of bulk materials and thin lms. Commercialized instrumentation
Table 8
Relative combined uncertainty of indentation properties for the micro and macro
range. After [65].
Property
Martens hardness, HM
Martens hardness from slope
of loading curve, HMs
Indentation hardness, HIT
Indentation modulus, EIT
Macro range,
100 N
67
820
34
517
68
68
35
46
Pilot participants.
813
Table 10
Maximum indentation forces for calibration and test piece.
Group
Low force
High force
0.1, 0.5, 1, 5, 10
10, 50, 100, 500, 1000
0.1, 1, 5
10, 50, 100
data for both ranges. Table 10 shows the maximum forces used for
the calibrations in tungsten and fused silica, and for the
measurements of hardness and elastic modulus of the (1 0 0)
aluminum test piece.
The loading function shown in Fig. 3 was prescribed in the
protocol and used by all participants. The loading function
consisted of: a 30 s loading, a 30 s hold at the maximum force,
unloading to 10% of the maximum force in 10 s, a 60 s hold at 10%
of the maximum force and a 2 s unloading to zero force. The drift
rate of the instrument was either determined from the last 50 s of
the hold period at 10% of the maximum force or prior to the start of
the indentation cycle. If the drift rate exceeded 0.1 nm/s the
indentation was excluded from the data set. A Berkovich diamond
indenter was used for all indentations. Ten indentations were
performed for each maximum load for both the calibrations and
the test piece measurement. The participants were asked to report
the plane strain indentation modulus, the indentation hardness
and the Martens hardness obtained for the (1 0 0) aluminum test
piece. The plane strain indentation modulus, is related to the
indentation modulus, given in Eq. (3), by the following:
EIT
EIT
1 ns 2
(16)
F
AS hmax
(17)
Fig. 17. Indentation modulus, EIT, obtained for the (1 0 0)Al test piece over the range
of forces investigated. The dotted line represents the value of elastic modulus
obtained by laser acoustic measurements on similarly prepared (1 0 0)Al.
Fig. 18. Indentation hardness, HIT, obtained for the (1 0 0)Al test piece over the
range of forces investigated.
Fig. 19. Martens hardness, HM, obtained for the (1 0 0)Al test piece over the range of
forces investigated.
814
Fig. 20. Repeatability CV of (a) indentation modulus and (b) indentation hardness
over the range of test forces investigated. Also shown are the results from the 1997
CIRP intercomparison on steel.
Fig. 21. Reproducibility CV of (a) indentation modulus and (b) indentation hardness
over the range of test forces investigated. Also shown are the results from the 1997
CIRP intercomparison on steel.
Table 11
Repeatability CV obtained for indentation modulus and indentation hardness for a range of materials and test forces.
Test force (mN)
Indentation modulus
Indentation hardness
(1 0 0)Al [42]
Ni [38]
Steel [77,78]
Glass [77,78]
BK-7 [38]
(1 0 0)Al [42]
Ni [38]
Steel [77,78]
Glass [77,78]
BK-7 [38]
0.1
1
5
10
50
100
0.14
0.09
0.09
0.07
0.05
0.05
0.04
0.01
0.15
0.12
0.20
0.18
0.12
0.10
0.07
0.10
0.02
0.01
0.31
0.13
0.10
0.08
0.03
0.02
0.03
0.01
0.20
0.17
0.16
0.14
0.55
0.22
0.11
0.08
0.05
0.02
0.01
s IT
1 F max
c Ac
eIT a tan g
815
(20)
where a 0.2% offset strain has been assumed. The yield strength can
then be calculated from this strain. The indentation tensile
strength, su,IT, can be calculated by setting eu = nIT in the equation:
s u;IT K eu nIT
(21)
816
Table 12
Comparison of methods for the derivation of tensile test properties from IIT [39].
Method 1: Representative stress and strain
Computational simulation
Experiments
Analysis
6 metals in [81]
7 metals in [83]
2 metals in [82]
Round-robin test (RRT) completed
in Korea
2
5
4
6
Relative advantages
Deterministic algorithm
No need for computational simulations
Sufcient experimental verication
Relative disadvantages
Rigid algorithm
Indispensable determination of
starting parameters
Fig. 22. Viscoelasticplastic model with spring, plastic element, dashpot, and two
KelvinVoigt bodies. C0, C1, C2 are compliances, E0 and H0 are instantaneous elastic
modulus and hardness, Y is yield strength, hv is viscosity, cv is viscous compliance
and t1, t2 are retardation times [97].
metals in [89]
metals in [88]
metals in [90]
ceramic and coating [86]
3 metals in [92]
4 metals in [93]
t1
t2
Fig. 23. Test force vs. time cycle for the indentation of viscoelasticplastic materials
such as biological materials.
cv tR
C1 C2
2
(23)
(24)
817
(26)
Fig. 24. Model of indentation test machine and test piece used in the analysis of
dynamic indentation. After [100].
Fig. 25. Photograph of dragony Anax parthenope julius Brauer (a) and detailed view
of the stigma (b). The location of the stigma on the wing of the dragony in (a) is
denoted by a rectangle. Location of indentations given by numbers. After [107].
818
6. Conclusions
We have presented a review of the measurement methods used
in nanoindentation, the instruments currently in use, and the
procedures for the analysis of the resulting data. The methods
developed for verication and calibration, including a discussion
on uncertainty of parameters were presented. The results of the
most recent CIRP sponsored comparison on nanoindentation were
presented and compared to the results obtained in the rst such
comparison. Two examples of some emerging uses of the
technique, namely determination of materials tensile properties,
and investigations of biological materials were discussed.
Although the ISO standards for the instrumented indentation
testing of bulk materials were published in 2002, it is still not
uncommon to nd published papers that do not follow the
standards. The use of the standards in the 2009 CIRP sponsored
comparison on nanoindentation contributed to the improvement
of reproducibility in the measurement of the indentation modulus
and indentation hardness when compared to the results of the
1997 CIRP sponsored comparison. In the emerging areas of
instrumented indentation for the derivation of material tensile
properties and the testing of biomaterials, currently no standards
exist, however work on developing standards in these areas is ongoing. With the adoption of standards in these emerging areas
improvements in the reproducibility of results are expected.
Acknowledgements
The authors would like to thank Drs. R. Hocken, G. Goch, W.T
Estler, K.-D. Bouzakis, Yu. Golovin, T. Chudoba and all those who
have provided materials for and thoughtful review of this
contribution. We would also like to thank the participants in
the recent CIRP sponsored comparison for their signicant efforts
to make it a fruitful exercise. We thank the University of North
Carolina at Charlotte and the PTB in Braunschweig for assistance
with the comparison. Additional thanks are extended to the
ofcers of the CIRP Scientic Technical Committee STC S, Drs. A.
Balsamo, H. Hansen and H. Haitjema for their help and support of
this work.
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