Middle East Technical University

Department of Mechanical Engineering

ME 498 Mechanical Characterization of Materials

6. Nanoindentation and Nanoscratch

 Nanoindentation
• Nanoindentation is a small scale version of classical indentation hardness measurements.
• A three-sided pyramid diamond tip is pushed on the specimen surface.
• Force and displacement is controlled with nN and sub-nm resolution.
• Hardness and elastic modulus of the material can be determined by analyzing the force
displacement curve.
coil

magnet

springs

capacitance
displacement indenter
gage

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 Berkovich Tips
• Berkovich is the most commonly used geometry for nanoindentation.
• Spherical, conical and cube corner tips can also be used.

AFM Image of a 3 µm deep indentation on

http://bm3.unl.edu/hysitron-nanoindenter Cu90Nb10 alloy (Özerinç et al. 2011)

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 Load – Displacement Curve

max

A schematic representation the specimen

cross-section during and after indentation
(Oliver and Pharr 1992).

hf: permanent indentation depth after removal of the force

hc: is the depth of contact of the indenter at Fmax (briefly named as depth of contact)
hmax: indentation depth at Fmax

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 Nanoindentation Hardness
• Nanoindentation hardness is defined as the maximum force applied divided
by the projected area of the contact at the maximum load.
• Hardness and elastic modulus is commonly determined by the Oliver-Pharr
method developed in 1992.

𝐹𝑚𝑎𝑥
𝐻= 𝐴𝑝 = f(ℎ𝑐 )
𝐴𝑝
Fmax is directly measured during nanoindentation.
Ap is a function of hc and unfortunately hc cannot
be measured directly.

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 Contact Depth, hc
Contact depth is calculated as the x-intercept of
stiffness tangent going through Fmax.
ℎ𝑐 = ℎ𝑚𝑎𝑥 − ℎ𝑠
where hs is the deflection of the specimen
surface adjacent to the nanoindenter.

𝐹𝑚𝑎𝑥
ℎ𝑐 = ℎ𝑚𝑎𝑥 − 𝜀
𝑆
ε is a geometric constant.
S is the surface stiffness at the top of the
unloading curve, which corresponds to the slope
of the force-displacement curve at that point.
2 max
𝜀= 𝜋 − 2 for a Berkovich tip.
𝜋

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 Contact Stiffness, S

Unloading in nanoindentation does not result

in a linear curve due to the nonlinear
geometry.
Therefore, a power-law curve fit is applied on
the top part of the unloading curve:
𝐹 = 𝑘(ℎ − ℎ𝑓 )𝑚
where k and m are least squares fitting
parameters. Then the stiffness becomes,
𝑑𝐹 𝑚−1
𝑆= ቤ = 𝑘𝑚 ℎ − ℎ𝑓
𝑑ℎ ℎ ℎ𝑚𝑎𝑥
𝑚𝑎𝑥
and the contact depth is,
Note: Typically, the curve fit is applied
𝐹𝑚𝑎𝑥 by excluding the bottom 20% and top
ℎ𝑐 = ℎ𝑚𝑎𝑥 − 𝜀 5% of the unloading curve.
𝑆

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 Projected Contact Area, Ap
𝑙 3
𝑡𝑎𝑛600 = 𝑙= 𝑎
𝑎/2 2

𝑎𝑙 3 2
𝐴𝑝 = = 𝑎
2 2
ℎ𝑐
𝑐𝑜𝑠65.270 =
Projected 𝑏
area
𝑎𝑐𝑜𝑠65.30
ℎ𝑐 = 𝑎 = 2 3ℎ𝑡𝑎𝑛65.30
2 3𝑠𝑖𝑛65.30

𝐴𝑝 = 3 3ℎ2 𝑡𝑎𝑛2 65.30 =24.56ℎ𝑐2

𝐹𝑚𝑎𝑥
𝐻=
𝐴𝑝

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 Elastic Modulus
• Nanoindentation also provides the elastic modulus. First step is the calculation
of the reduced modulus:
( 𝜋 ∙ 𝑆)
𝐸𝑟 =
2𝛽 𝐴𝑝
• 𝛽 is a constant that depends on indenter geometry (1.034 for Berkovich tips).
• Reduced modulus includes the combined effects of the elastic deformation of
the specimen and the diamond tip:
1 1 − 𝜈𝑠2 1 − 𝜈𝑖2 1 − 𝜈𝑠2
= + 𝐸𝑠 =
𝐸𝑟 𝐸𝑠 𝐸𝑖 1 1 − 𝜈𝑖2
𝐸𝑟 − 𝐸𝑖
𝐸𝑖 = Elastic modulus of the indenter (1141 GPa for diamond)
𝐸𝑠 = Elastic modulus of the sample
𝜈𝑖 = Poisson’s ratio of the indenter (0.07 for diamond)
𝜈𝑠 = Poisson’s ratio of the sample

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 Continuous Stiffness Measurement

• A conventional nanoindentation at a
single location provides one hardness and
elastic modulus value.
• A more recent technique called CSM
enables the continuous measurement of
hardness and elastic modulus as a
function of penetration depth.
• The formulation is mostly the same, but
stiffness S, is measured continiously by
Example data showing the
oscillating the indenter tip with a small
hardness of a metallic film on
amplitude around 1 nm. a hard substrate. (Özerinç et
• Tip oscillation and associated forces can al. 2018, unpublished work)
be analyzed to obtain the stifness, using a
mass-spring-damper model.

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 Experimental Effects: Surface Roughness
• The Oliver-Pharr analysis assumes a perfectly sharp diamond indenter on a
perfectly smooth surface.
• Any surface irregularity will change the mechanical response and result in error.
• ISO standard states that the surface roughness should be smaller than 5% of the
indentation depth.

Indentations on a smooth and a rough

surface

Figures taken from the presentation of Dr. Phillippe Kempe, Anton Paar 11
 Experimental Effects: Substrate

Stress field below the indenter tip can remain significant at depths up to ten times
the indentation depth.
ℎ𝑚𝑎𝑥
For thin films on a substrate, it is recommended that ≤ 0.1
𝐹𝑖𝑙𝑚 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠

Hfilm ≈ 5.5 GPa

Hardness of 1 µm Hsubstrate ≈ 9 GPa

Cu90Nb10
nanocrystalline film
on SiO2 substrate.

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 Other Experimental Aspects
Diamond tips are not perfectly sharp. They can also get dirty and show some wear.
Indentations should be performed on silica specimens of known elastic modulus for
calibration.

deviation from ideal

due to finite tip radius

hardness of ideal tip

Modified area function for a non-perfect tip:

Özerinç, data taken in UIUC in 2011 13

 Other Experimental Aspects (continued)
• Thermal drift would cause erroneous results and
temperature should be maintained constant in the
room.
• Vibration is not desirable and nanoindenters are
usually placed in a basement.
• Specimens should be handled with gloves to
prevent contamination.
• Tips can be cleaned by indenting on a soft metal
such as aluminum or by cleaning with acetone and
IPA.
• When a special mounting is required, the stiffness
of the frame should be recalibrated.
Acoustic enclosure of
Hysitron TI 980

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 Applications of Nanoindentation
Most of the applications fall into one of the below categories.
1) Specimen is small and cannot be tested by any other method.
2) Specimen is large and the mechanical behavior of the specimen at the
microscale is of interest.

AlTiN coatings for wear

resistance Indentation size effect in single crystal bulk
specimens, (Zhao et al. 2003).

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 Nanocrystalline and Nanolayered Materials
• We prepare 1 µm thick
nanolayered pure metal films.
• Layers are alternating with pure
copper and pure niobium, with
layer thicknesses in the range 5
nm – 100 nm.
100 nm
• We measure the hardness by
8
using nanoindentation.
• We observe that hardness 7
Cu90Nb10-Nb
increases with decreasing layer 6
thickness. Hardness (GPa)
5
• Also, when we add niobium to Cu-Nb
pure copper layers, strength 4
increases. This can be attributed Cu-Nb data from Misra 2009
3
to solid solution strengthening.
2
0 50 100
Layer Thickness (nm) 16
 Biomechanics Applications

Nanoindentation of tooth provides insight

to the mechanical properties of different
tissue.

Ebenstein et al. 2006 17

 Scratch Testing
• Scratch test is a method used to
investigate the hardness, cohesion and
adhesion properties of bulk materials
and coatings.
• The results provide information about
the scratch resistance of materials and
adhesion of the coatings to surfaces.
• A diamond tip is pushed onto the
specimen and the specimen is moved
along a line to generate a scratch on
the surface.
• Vertical force, lateral force, scratch
speed and penetration depth and
acoustic emission are measured.

Image from Hysitron.com

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 Scratch Test Types

•Scratch Hardness Test:

This technique uses a constant load scratch and provides
better differentiation of damage behavior. Such test
requires more specimens area and test time.

•Scratch Adhesion Test:

This technique uses a gradually increasing load in a single
scratch. Therefore, it is faster than Constant Load test and
commonly used for research.

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 Scratch Test Types and Example Parameters

• Scratch Hardness Test

This technique uses a constant load scratch and provides better differentiation of
damage behavior. Such test requires more specimens area and test time.
• Scratch Adhesion Test
This technique uses a gradually increasing load in a single scratch. Therefore, it is
faster than Constant Load test and commonly used for research.
• Example Parameters for a Linear Scratch Adhesion Test
4 mm/min scratch speed
4 mm scratch length
Rockwell Diamond Indenter with 100 µm diameter
Linearly increasing loading from 50 to 10,000 mN
Data acquisition rate of 10 Hz

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Data for the Scratch on a Metallic Thin Film on SiO2
Measured Fn (mN) Ft (mN) AE (arb. unit) COF

12 0.2

10 Coefficient of friction 0.15

8 Critical load

Scratch COF
Force (N)

0.1
Lc ≈ 4500 mN
6 Acoustic emission
0.05
4

2 0

0
Tangential force -0.05
0 Scratch Length
1 (mm) 2 3 4 5
0
1
Depth (µm)

Residual depth
2
3 Penetration depth
4 Pd (nm) Rd (nm)
5

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 Critical Load

• Lc is the critical load at which a specific,

well-defined, recognizable damage/failure
event occurs.
• At the critical point, there is usually an
abrupt change in the lateral force,
coefficient of friction, and acoustic
emission.
• When the type of failure changes,
additional critical loads are defined as
necessary, (Lc2, Lc3).

S. Kuiry, “Advanced Scratch Testing for Evaluation of Coatings ,” Bruker Nano Surfaces 23
Division, May 8, 2012, Presentation
 Optical In-Situ Scratch on a Diamond-like Carbon (DLC) Coating

There are 4 main stages

of deformation:
• Elastic surface
deflection
• Plastic deformation
of the coating
• Ring crack formation
• Compressive
spallation of the
coating ahead of the
indenter

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