Instructor: Yury Gogotsi

Indentation (Hardness) Test

Introduction to Load (P)

Indenter

Nano
Indentation Specimen

Hardness – resistance to penetration of a hard indenter

Acknowledgements: V. Domnich, T. Juliano, M. Barsoum

Hardness Introduction
Hardness is a measure of a material’s resistance to surface penetration by an
indenter with a force applied to it.
Hardness • Mechanical measurement
Brinell, 10 mm indenter, 3000 kg = Load F/surface area of indentation
in micro scale -
Microindentations
Vickers: Diamond pyramid indentation.
– To study the mechanical
Microhardness behavior of different
Vickers micro-indentation = size of pyramid comparable to orientations we need single
microstructural features. You can use to assess relative hardness of various crystals
phases or microconstituents. This is an optical photo of a Vickers – For a bulk sample it’s hard to
Nanoindentation indentation (98N) in silicon nitride. get a nano-scale response
The specimen is tilted to show the from different grains
three dimensional form of the
indentation, including the tip – Very little information on the
cracking and the side uplift elastic-plastic transition

http://moremetallography.com/ceramics/ceramics.htm

Introduction
• The depth-sensing nanoindentation method
gained popularity with the development of
– Machines that can record small load and
displacement with high accuracy and precision;
– Analytical models by which the load-displacement
data can be used to determine modulus, hardness
and other mechanical properties.
Micro- vs. Nano-Indentation
Microindentation
A prescribed load is applied to an indenter
in contact with a specimen and the load is d
then removed and the area of the residual
impression is measured. The load divided P
by the area is called the hardness. VH =
d2
Nanoindentation (depth-sensing indentation)
A prescribed load is applied to an indenter in contact
with a specimen. As the load is applied, the depth of
loading

Load (P)
penetration is measured. The area of contact at full P = α (h - hf)m
load is determined by the depth of the impression unloading
and the known angle or radius of the indenter. The
hardness is found by dividing the load by the area of
S
contact. Shape of the unloading curve provides a
measure of elastic modulus. hc hmax

Displacement (h)

Contours of principal normal stresses in

(a) Boussinesq and (b) Hertzian fields,
Schematic of the various types of shown in the plane containing contact axis
indenter tips used in indentation testing:
(a) Vickers, (b) Berkovich, (c) Knoop, (d)
σ11
conical, (e) Rockwell, and (f) spherical 0.0005
0.008
0.005
-0.500
-0.025
0.0002 0.005 0.007

-0.008
-0.100
-0.002 σ22 -0.025
0.008
0.0005 0
0.002 0.005

-0.002 -0.030
-0.100
-0.128 -0.008 σ33 -0.750
(a) (b) (c) (d) (e) (f) -0.250
-0.032

(a) (b)
 Tip Geometry - Berkovich
• Advantages:
– Sharp and well-
defined tip geometry
– Well-defined plastic
deformation into the
surface
– Good for measuring
modulus and
hardness values
• Disadvantages:
– Elastic-plastic
transition is not clear
http://www.bbt.admin.ch/kti/success/archiv/nano_micro/f/power.htm
Tip Geometry - Spherical
• Advantages:
– Extended elastic plastic
deformation
– Load displacement results
can be converted to
indentation stress-strain
plots
– Useful in determination of
yield point
• Disadvantages:
– Tip geometry is not very
sharp and the spherical
surface is not always
perfect
MTS Tech sheet for spherical tip

Testing Issues Surface Roughness

• Sample Issues
– Surface Roughness
– Inhomogeneities
• Contamination or oxide layers
• Multi-layered structure
• Thin films
• Gradient layers
• Multi-phase materials
• Materials that has particles embedded in them • Roughness has significant effect on mechanical
properties
• Machine Issues • A model can be developed to account for the roughness
– Machine compliance • Surface roughness should be significantly smaller in
– Tip shape function lateral dimension than the indenter tip
– Drift

http://www.nanoindentation.cornell.edu/
 Material Response to Intentation Analytical Models
surface profile after P
load removal • The basic assumptions of this approach are,
indenter Pmax – Deformation upon unloading is purely elastic
hs = ε
hr initial
surface – The compliance of the sample and indenter tip can be thought of as
S a combination of springs in series
1 1 − υi 1 −υs
2 2

= +
hc = hmax − hs
h Er Ei Es
hs hc surface profile
under load – The contact can be modeled as a rigid indenter of defined shape
with a homogeneous isotropic elastic half-space where stiffness, S
7 2 A
S=
A(hc ) = 24.5hc + ∑ C h
2 1/ 2i Er
Contact area: i c π
i =0 • The main challenge lies in the determination of the actual
contact area, A, at load.
P – applied force hc – contact depth
h – indenter displacement hr – plastic deformation after load removal
C - coefficient hs – surface displacement at the contact perimeter Sneddon, I.N., International Journal of Engineering Science, Vol. 3, p. 47, 1965
Pharr, G.M.; Oliver, W.C. and Brotzen, F.R., Journal of Materials Research, Vol. 7, No. 3, p. 613, 1992

Oliver & Pharr, J. Mater. Res. 1992

Analytical Models Analytical Models

• Field and Swain Approach:
They treated the indentation as a
reloading of a preformed
impression with depth hf into
reconformation with the indenter
4
P= E r R1 / 2 h 3 / 2
3
2/3
⎛ Pmax ⎞
h part ⎜ ⎟ − hend
hc ⎜P ⎟
hc hf = ⎝ part ⎠
2/3
⎛ Pmax ⎞
⎜ ⎟ −1
⎜P ⎟
• Doerner-Nix Model: ⎝ part ⎠

Pmax ⎛ hend + h f ⎞
2

Ac = f (hc ) H=
Ac
a = R(hend + h f ) − ⎜⎜
⎝ 2
⎟⎟
⎠

Doerner, M.F. and Nix, W.D., Journal of Materials Research, Vol. 1, No. 4, p. 601, 1986 Field, J.S. and Swain, M.V., Journal of Materials Research, Vol. 8, No. 2, p. 297, 1993
Fischer-Cripps, A. C., Vacuum 58 (2000), 569-585
 Continuous Stiffness
Analytical Models
• Oliver and Pharr Model:
Measurement
• The nanoindenter system
applies a load to the indenter tip
to force the tip into the surface
while simultaneously
superimposing an oscillating
P = α (h − h f ) m force with a force amplitude
generally several orders of
magnitude smaller than the
nominal load.
P
hc = ht − ε • It provides accurate
S measurements of contact
stiffnesses at all depth.
Ac = f (hc ) • The stiffness values enable us
to calculate the contact radius at
Displacement, h any depth more precisely.

Oliver, W.C. and Pharr, G.M., Journal of Materials Research, Vol. 7, No. 6, p. 1564, 1992 Oliver, W.C. and Pharr, G. M., J. Mater. Res., 19 (1), Jan 2004
Bhusan, B. and Li, X., Materials Characterization 48 (2002), 11-36

How are Stiffness, Hardness and

Load vs. Displacement
Modulus Calculated?
Pmax Pmax
Stiffness = (dP/dh)h=hmax (N/m)
Hardness = Maximum Load / Projected
Pmax
Contact Area at Maximum Load = Elastic Plastic
Pmax/Aproj (Pa)
hr = 0 hr = hmax
Modulus → Two key equations:

Load, P
Load, P

1 1 −ν 2 1 −ν i
Load, P

2
πS
Er = = +
2 β A proj Er E Ei
β=1 for circular contact, 1.034 for
Berkovich and cube corner
ν is estimated/known, Aproj is calibrated,
and E is solved for hmax
hmax
S 0
Displacement, h 0 Displacement, h
Displacement, h Er – reduced modulus of elasticity
Ei – modulus of elasticity of indenter
 Energy Considerations
Elastoplastic Material
Elastic energy
Loading
P = α1h2 Ue = 1 α 2hmax
3
(1- ξr )3
3
Loading Unloading Unloading
Hysteresis loop energy
P = α1hm P = α2(h-hr)m P = α2(h-hr)2

Load, P
Ur = 1 α1hmax
3
ξr
Load, P

Analytical solution Work of indentation

m = 1 for flat cylinders Ur

WI =
Vr
m = 2 for cones
m = 1.5 for spheres Ur Ue with ξ r ≡ hr = 1-
α1
hmax α2

0 hf hmax Vr 1 gh 3
ξ
0
3 max r
Displacement, h
Sneddon, Int. J. Engng. Sci. 1965 Displacement, h
Sakai, J. Mater. Res. 1999

Nano Indenter XP® (MTS Systems)

A Wealth of Different Machines
Micro Photonics CSM Nano
Hardness Tester
• Maximum applied load is
500 mN
• Indenter load resolution of
50 nN, and displacement
resolution of <.02 nm
• Obtains reliable
characterization data for thin
films and individual grains
• Testworks 4 software is
used for analysis of
collected data
• Scratches can be made
CSIRO Ultra-Micro Hysitron Triboindenter
with this machine
Indentation System
 Indenter Tips: Pyramidal
Nanoindentation Systems Berkovich
The total included angle on this tip is
142.3°, with a half angle of 65.35°. This
load frame makes it a very flat tip. This tip geometry
has been used as the standard form
loading
actuator nanoindentation. This tip is used primarily
for bulk materials and thin films greater
load sensor than 100nm thick. The average radius of
load train curvature for a Berkovich tip is typically
between 100nm and 200nm.
displ. indenter
sensor specimen Cube Corner (90 degree)
sample The total included angle of this tip is 90°
holder and has the same shape as the corner
of a cube. Because it has sharper
angles and a higher aspect ratio, the
radius of curvature can be much smaller
than that for a Berkovich tip. These tips
Controlled loading. Depth resolution <1nm specialty is ultra thin films, where plastic
deformation should be kept to a more
confined volume.

Indenter Tips: Sphero-Conical

SEM image of a typical nanoindentation
in GaAs Radius 1 – 3 µm
These tips can be used for indentation & scratch
[Berkovich tip; 50 mN loading; (111) testing. Samples that would need these for
indentation may include polymers that are too soft
surface]. to image with Berkovich tips. Because of the non-
directional geometry at the end of these tips, they
are good scratching tips for harder materials,
GaAs where plastic deformation is desired. For ultra thin
films, it may be best to have a cube corner tip for
scratching.

Radius 3 – 200 µm
These tips are used for indenting in very soft
materials. Samples may include very soft polymers
and biological samples. They are also good for
scratching on harder materials when no plastic
1 µm
deformation is desired (e.g. to find coefficient of
friction).
 Pile-up and Sink-in
Point-Force Indentation
Loading geometry Load-displacement curve

Spherical Indentation Conversion to Stress-Strain ‡

4
Loading geometry Load-displacement curve P= E r Rhe3
3
P
hc = ht − 0.75
S

a= 2Rhc − hc
2

hs
P
σ=
c MTS Nanoindenter πa 2
c hs with Continuous
Stiffness Measurement Strain = a/R
 Choosing an Appropriate Indenter
Sharp indenters:
Characteristic strain is constant
regardless of the load or displacement.
Thus, the sharper the cone or pyramid,
the larger the characteristic strain. To
obtain the stress-strain relationship of a
material, multiple tests using indenters
with different included angles is
required.
Spherical indenters:
Characteristic strain changes
continuously as the indenter penetrates
into material. In principle, one can
determine the elastic modulus, yield
stress, and strain-hardening behavior of
a material all in one test.
Machine Stiffness Calibration
Using an accurate value of
machine stiffness is very
important for large contacts,
where it can significantly affect
the measured load-
displacement data.
ε = 0.2 cot (ψ)
ψ – included angle of the indenter
0.2 a
ε=
R
a – radius of contact
R – radius of the indenter
Usually done by manufacturer
using materials with known
properties (aluminum for large
penetration depths, fused silica
for smaller depth).
Machine Compliance
• Displacement arising from the compliance of the testing machine
must be subtracted from the load-displacement data
• The machine compliance includes compliances in the sample and
tip mounting and may vary from test to test
• It is feasible to identify the machine compliance by the direct
measurement of contact area of various indents in a known material
• Another way is to derive the machine compliance as the intercept of
1/total contact stiffness vs. 1/sqrt(maximum load) plot, if the Young’s
modulus and hardness are assumed to be depth-independent.
Oliver, W.C. and Pharr, G.M., Journal of Materials Research, Vol. 7, No. 6, p. 1564, 1992
Thermal Drift
• Drift can be due to vibration or a thermal drift.
• Thermal drift can be due to
– Differential thermal expansion in the machine
– Heat generation in the electronic devices
• Drift might have a parallel and/or a perpendicular
component to the indenter axis
• Thermal drift is especially important when studying time
varying phenomena like creep.
Oliver, W.C. and Pharr, G.M., Journal of Materials Research, Vol. 7, No. 6, p. 1564, 1992
 Thermal Drift Calibration Real Indenter Tips:
Indenter displacement vs. time
Deviation from Perfect Shape
during a period of constant
load. The measured drift rate,
0.31 nm/s, is used to correct
the load-displacement data

Application of thermal
drift correction to the Radius 100 µm Radius 1 µm
indentation load-
displacement data Sphero-Conical

Area Function Calibration Thin Films: NiP on Copper

Ideal tip geometry yields the
following area-to-depth ratio:

A = 24.5 hc2

Real tips are not perfect !

Calibration:
Use material with known
elastic properties (typically,
fused silica) and determine its
hc2 area as a function of contact
depth. Then fit the
experimental data to the
(hc) expression

A = C1hc2 + C2hc + C3hc1/2 + C4hc1/4 + C5hc1/8 + …

Now, use the new area tip function for all measurements.
Contact areas (dashed lines) and contact stresses at the interface Typical Load-Displacement Curves in
of the regular tetrahedral pyramid penetrating into the half-space. Nanoindentation Experiments
The maximum contact stresses are observed in the center of
indentation zone and decrease according to the stress isobars
(solid lines). (a) Stress singularities in the purely elastic loading
pop-out
and (b) their reduced form when the non-linearity of the half-space 40
is taken into account.
most 20
elastoplastic
0
materials
elbow
40

Load, mN
P
20

0
elbow & pop-out
40
silicon 20
(a) (b)
0
h 0 100 200 300 400 500
Displacement, nm

Effect of Phase Transformations the Shape

of Indentation Curves Raman Analysis of
15
Nanoindentations in Silicon
40 pop-out
10
20
5 Nano-
Average Contact Pressure (GPa)

Analysed spot Pristine Si

0
0
6 GPa indentation
Applied load (mN)

elbow 15
40 Si-I (cd)
10 350
Si-III (bc8)
20 4 GPa 433
5 Si-XII (r8)
394
0 382
0
521
elbow & 15 500 nm
40
pop-out 10 166
20 520
5 - (111) polished Si wafer
0 5 GPa - 50 mN max load
0
0 200 400 200 400
- 3 mN/sec loading rate
200 400 600 200 400 600
Displacement (nm) Contact Depth (nm) Wavenumber, cm-1
 Application of Quasi-static
Creep Measurement
Nanoindentation
• Plastic deformation in all
materials is time and
Si II temperature dependent
• Important parameter to
determine is the strain rate
sensitivity
• The average strain rate can be
Si I
given by
1 dhc
.
ε ind =
Si III and Si XII hc dt
• It can be done by experiments
at different loading rates or by
studying the holding segment of
a nanoindentation

Juliano, T., Domnich, V. and Gogotsi, Y., J. Mater. Res. 19[10], 2004 Mayo, M.J. and Nix, W.D., Strength of Metals and Alloys, Proceedings of the 8th International
Conference on the Strength of Materials, p. 1415, 1988

Example of Creep Measurement

Poly Tetra-Fluoro Ethylene
Fatigue Measurement
• Nanoscale fatigue has not
been studied extensively
because of lack of
instruments.

• CSM can provide sinusoidal

force cycles at high
frequencies.

• Change in contact stiffness

can give us fatigue behavior
as contact stiffness is
sensitive to damage
formation.

Bhusan, B. and Li, X., Materials Characterization 48 (2002), 11-36 Bhusan, B. and Li, X., Materials Characterization 48 (2002), 11-36
 Case Stusy: in vitro interfacial mechanics of a
Example of Nano-fatigue bioactive composite
Measurement (Silicon) A bioactive composite of hydroxyapatite (HA) and polymethyl-
methacrylate (PMMA), with an addition of a co-polymer coupling
agent was examined for a mandible replacement. The influence of
the coupling agent on the local mechanical properties of the system
before and after in vitro immersion conditions was determined via the
application of nano-indentation onto the interface between HA and
PMMA of the cross-section of the composite. The fracture
mechanism and position of each indent mark was analyzed at up to
5000x magnification under field emission environmental scanning
electron microscopy. Coupling the microscopic analysis with the load-
displacement curve provided a more comprehensive local analysis
than has previously been accomplished. The in vitro mechanical
properties of the HA particulates showed a reduction of bulk bending
properties, local elastic modulus and local hardness with increase of
immersion time. While the coupling agent improved the interfacial
mechanical properties up to 72 hours immersion, it did not affect the
surface bioactivity of the system as shown in the measurement of
Bhushan, B. and Li, X., Surface and Coatings Tech., 163-164(2003), 521-526 calcium and phosphate concentration uptake.
Emily Ho &. Michele Marcolongo, Drexel U

Nano indentations on Bioactive Composites

Biocomposite
To determine the local mechanical properties of
• Human bone: a bioactive composites a function of immersion
– 45 - 60 % mineral: Hydroxyapatite period in simulated body fluid (SBF).
– 20 - 30 % matrix: collagen
– 10 - 20 % water

(a) salt (b)

• New Bone replacement material:
– Ceramic (reinforcement) + polymer (matrix)

Polymer matrix: Polymethylmethacrylate

indentation
Ceramic filler: Synthetic Hydroxyapatite
indentation

FE-SEM photos of the 72 hours SBF immersed composites with indentations at:
(a) the center of the bioactive ceramics particle (3500x) and
(b) the ceramics/polymer interface (5000x).
The “in vitro” Local Mechanical Properties of the Bioactive
Composites as a Function of Surface Bioactivity Summary
• Nanoindentation is an important technique to determine various
Controls mechanical properties of a material in nanoscale
12
• The continuous stiffness measurement or dynamic indentation
Un-immersed method is useful in measuring contact stiffness, elastic modulus,
10 72 hours
immersed
hardness, creep resistance and fatigue properties of the materials
8 • CSM probes the mechanical property changes in situ during
indentation
Load [mN]

6
• CSM indentation creep tests can detect creep displacement and
4 stress relaxation at small volumes
• Nanoscale fatigue tests are important for applications like MEMs
2
and magnetic storage devices
0 • Future versions of dynamic nanoindenters should have the
0 100 200 300 400 500 600 700
capability of measuring at a wide frequency range and also some
Displacement [nm]
models has to be developed to account for viscoelasticity

Nanomechanical Testing
Nanoindentation Testing
Suggested reading:

Tests Common Applications Fischer-Cripps, A.C., "A review of analysis methods for sub-micron indentation
testing," Vacuum, 58, 569-585 (2000).
• Fracture Analysis
• NanoHardness/ Elastic Modulus Hay, J.L. and Pharr, G.M., "Instrumented indentation testing," Mechanical
• Anti-Wear Films
• Continuous Stiffness Measurements Testing and Evaluation, eds. Kuhn, H. and Medlin, D., ASM International
• Lubricant Effects
• Acoustic Emissions (2000).
• Paints & Coatings
• Properties at Various Temperatures
• Nanomachining
• Friction Coefficient Baker, S.P., "Between nanoindentation and scanning force microscopy:
• Bio-materials
• Wear Tests measuring mechanical properties in the nanometer regime", Thin Solid
• Metal-Matrix Composites
• Adhesion Films, 308-309, 289-296 (1997).
• Diamond Like Carbon Coatings
• NanoScratch Resistance
• Semiconductors
• Fracture Toughness
• Polymers
• Delamination
• Thin Film Testing & Development
• Property/ Processing Relationships
 Nanopatterning of Si Wafers

10 µm

Optical images of Berkovich

40 µm nanoindentations on Si, 50
mN load.

Through control of loading conditions, amorphous silicon, Si-III (bc8),

and Si-XII (r8) phases with different electronic and optical properties
can be produced. Patterns of spots with varying shape or lines can
be readily repeated indefinitely.