Nanoindentation

Lecture 1 Basic Principle

Do Kyung Kim

Department of Materials Science and

Engineering
KAIST, Korea
Indentation test (Hardness test)

• Hardness – resistance to penetration of a hard

indenter
Hardness

• Hardness is a measure of a material’s resistance to

surface penetration by an indenter with a force
applied to it.

• Hardness
– Brinell, 10 mm indenter, 3000 kg Load F /surface
area of indentation A
– Vickers, diamond pyramid indentation

• Microhardness
– Vickers microindentation : size of pyramid
comparable to microstructural features. You can
use to assess relative hardness of various phases
or microconstituents.

• Nanoindentation
Microindentation

• Mechanical property
measurement in micro-
scale
(Micro-indentation)

– To study the
mechanical behavior of
different orientations,
we need single
crystals.
Optical micrograph of a Vickers – For a bulk sample, it is
indentation (9.8 N) in soda-lime glass
hard to get a nano-
including impression, radial cracking,
and medial cracking fringes.
scale response from
different grains.
– Very little information
on the elastic-plastic
transition.
Nanoindentation

• Nanoindentation = The depth sensing indentation =

The instrumented indentation

• 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 appled to an
indenter in contact with a specimen
and the load is then removed and the
area of the residual impression is
measured. The load divided by the by
the area is called the hardness.

• Nanoindentation
A prescribed load is appled to an
indenter in contact with a specimen.
As the load is applied, the depth of
penetration is measured. The area of
contact at full load is determined by
the depth of the impression and the
known angle or radius of the
indenter. The hardness is found by
dividing the load by the area of
contact. Shape of the unloading curve
provides a measure of elastic
modulus.
Schematics of indenter tips

Vickers Berkovich Knoop Conical Rockwell Spherical

Indenter geometry
Geometr
Semi Effective y
Indenter angle Intercep
Projected area cone angle correctio
type t factor
(θ) (α) n factor
(β)
Sphere A ≈ π2Rhp N/A N/A 0.75 1

Berkovich A = 3hp2tan2θ 65.3 ° 70.2996 ° 0.75 1.034

Vickers A = 4hp2tan2θ 68 ° 70.32 ° 0.75 1.012

A = 2hp2tanθ1tan θ1=86.25
Knoop 77.64 ° 0.75 1.012
θ2 ° θ2=65 °

Cube Corner A = 3hp2tan2θ 35.26 ° 42.28 ° 0.75 1.034

Cone A = πhp2tan2α α α 0.72 1

Stress field

Boussinesq fields Hertzian fields

Sharp indenter (Berkovich)

• Advantage
– Sharpt and well-
defined tip geometry
– Well-defined plastic
deformation into the
surface
– Good for measuring
modulus and hardness
values

• Disadvantage
– Elastic-plastic
transition is not clear.
Blunt indenter - Spherical

• Advantage
– Extended elastic-
plastic deformation
– Load displacement
results can be
converted to
indentation stress-
strain curve.
– Useful in
determination of yield
point

• Disadvantage
– Tip geometry is not
very sharp and the
spherical surface is
not always perfect.
Data Ananlysis

• P : applied load
• h : indenter displacement
• hr : plastic deformation after load removal
• he : surface displacement at the contact
perimeter
Analytical Model – Basic Concept

• Nearly all of the elements of this analysis were first developed by workers
at the Baikov Institute of Metallurgy in Moscow during the 1970's (for a
review see Bulychev and Alekhin). The basic assumptions of this approach
are
– Deformation upon unloading is purely elastic
– The compliance of the sample and of the indenter tip
can be combined as springs in series

– The contact can be modeled using an analytical model

for contact between a rigid indenter of defined shape
with a homogeneous isotropic elastic half space using

• where S is the contact stiffness and A the contact area. This relation was
presented by Sneddon. Later, Pharr, Oliver and Brotzen where able to show
that the equation is a robust equation which applies to tips with a wide
range of shapes.
Analytical Model – Doerner-Nix Model
Analytical Model – Field and Swain

• They treated the indentation as a reloading of a

preformed impression with depth hf into
reconformation with the indenter.
Analytical Model – Oliver and Pharr
Continuous Stiffness Measurement (CSM)

• The nanoindentation
system applies a load to
the indenter tip to force the
tip into the surface while
simultaneously
superimposing an
oscillating force with a
force amplitude generally
several orders of
magnitude smaller than the
nominal load.
• It provides accurate
measurements of contact
stiffness at all depth.
• The stiffness values enable
us to calculate the contact
radius at any depth more
 Analysis result

1 1 − υ 2 1 − υ '2
• Reduced modulus *
= + E: modulus of specimen
E’: modulus of indenter
E E E'

dP A
• Stiffness = 2E *
dh p

2 2
• Contact area A = 3 3h p tan 2 65.3 = 24.5h p

P
• Hardness H= 2
24.5h p

dP 1 1 π
• Elastic modulus E =
*
β = 1.034for Berkovich indenter
dh 2h p β 24.5
Material response
Analytical Model - ETC

• Elasto-plastic materials
Analytical Model - ETC

• Energy consideration
Nanoindenter tips
Berkovich indenter

l
tan 60 o =
a/2
3
b l= a
2
al 3 2
Aproj = = a
2 4
h
cos 65.27 o =
b
Projected area
a cos 65.3o a
h= =
2 3 sin 65.3o 2 3 tan 65.3o

a = 2 3h tan 65.3o

Aproj = 3 3h 2 tan 2 65.3o = 24.56h 2

Berkovich vs Vickers indenter
• Berkovich projected area • Vickers projected area

Aproj = 3 3h 2 tan 2 65.3o = 24.56h 2 Aproj = 4h 2 tan 2 68o = 24.504h 2

• Face angle of Berkovich indenter: 65. 3 °

• Same projected area-to-depth ratio as Vickers indenter

A = πh p tan 2 α
• Equivalent semi-angle for conical indenter: 70.3 ° 2
Commercial machines
• MTS_Nano-Indenter • CSIRO_UMIS
XP •(Ultra-Micro-Indentation
System)

• Hysitron_Triboscope • CSM_NHT
•(Nano-Hardness Tester)
 Commercial machine implementation
• MTS_Nano-Indenter • CSIRO_UMIS

• Inductive force generation system • Load via leaf springs by expansion of load actuato
• Displacement measured by capacitance gage • Deflection measured using a force LVDT

• Hysitron_TriboScope • CSM_NHT

• Two perpendicular transducer systems • Force applied by an electromagnetic actuator

• Displacement of center plate capacitively measured
• Displacement measured via a capacitive system
 Force actuation
• Electromagnetic • Electrostatic
actuation actuation

• most common means • Electrostatic force btwn 3-plate transducer applied

• long displacement range & wide load range• Small size (tenths of mm) & good temperature stability
• Large and heavy due to permanent magnet• Limited load(tenths of mN) & displacement(tenths of µN

• Spring-based force • Piezo/spring

actuation actuation

• Tip attached to end of cantilever & • Tip on leaf springs are displaced by piezoelectric actuat
• Sample attached to piezoelectric actuator • Force resolution is very high ( pN range),
• Displacement of laser determine displacement
• As resolution goes up, range goes down & Tip rotation
 Displacement measurement
• Differential capacitor • Optical lever method

ε ⋅ε0 ⋅ A
C=
d

• Measure the difference btwn C1 and C2 due to ∆ • Photodiode measures lateral displacement
• Popular method in cantilever based system
• High precision(resolution < 1 Å) & small size
• Relatively small displacement range • Detection of deflection < 1 Å

• Linear Variable • Laser interferometer

Differential Transducer
(LVDT)

• AC voltage proportional to relative displacement • Beam intensity depends on path difference

• High signal to noise ratio and low output impedance
• Sensitivity < 1 Å & used in hostile environment
• lower resolution compared to capacitor gage • Fabry-Perot system used for displacement detectio
Factor affecting nanoindentation

• Thermal Drift
• Initial penetration depth
• Instrument compliance
• Indenter geometry
• Piling-up and sinking-in
• Indentation size effect
• Surface roughness
• Tip rounding
• Residual stress
• Specimen preparation
Thermal drift

• Drift can be due to vibration or a thermal drift

• Thermal drift can be due to

– Different thermal expansion in the machine
– Heat generation in the electronic devices

• Drift might have parallel and/or a perpendicular

component to the indenter axis

• Thermal drift is especially important when studying

time varying phenomena like creep.
Thermal drift calibration

Indenter displacement vs time

during a period of constant
load. The measured drift rate
is used to correct the load
displacement data.

Application of thermal
drift correction to the
indentation load-
displacement data
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

• Anther 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
Machine compliance calibration

Usually done by manufacturer

using materials with known
properties (aluminum for large
penetration depths, fused
silica for smaller depth).

Using an accurate value

of machine stiffness is
very important for large
contacts, where it can
significantly affect the
measured load-
displacement data.
Real tip shape

• Deviation from perfect shape

Sphero-Conical tips
Area function calibration

• 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
• New area function its area as a function of
contact
A = C1hc2 + C2hc + C3hc1/2 + C4hc1/4 + C5hc1/8 + …
Surface roughness

• As sample roughness does have a significant effect on the

measured mechanical properties, one could either try to
incorporate a model to account for the roughness or try to use
large indentation depths at which the influence of the surface
roughness is negligible.
• A model to account for roughness effects on the measured
hardness is proposed by Bobji and Biswas.
• Nevertheless it should be noticed that any model will only be able
to account for surface roughnesses which are on lateral
dimensions significantly smaller compared to the geometry of the
indent
Pile-up and Sinking-in
Phase transition measurement

• Nanoindentation on silicon and Raman analysis

Creep measurement

• Plastic deformation in
all materials is time and
temperature dependent

• Important parameter to
determine is the strain
rate sensitivity

• The average strain rate

can be given by
1 dhc
ε ind =
hc dt
• It can be done by experiments at different
loading rate or by studying the holding segment
of a nanoindentation.
Fracture toughness measurement

Combining of Laugier proposed toughness

model and Ouchterlony’s radial cracking
modification factors, fracture toughness
can be determined.

Fracture toughness expression

Kc = 1.073 xv (a/l)1/2 (E/H)2/3 P / c3/2

Fatigue measurement

• Nanoscale fatigue has not

been studied extensively
because of lack of
instruments.

• CSM can provides

sinusoidal force cycles at
high frequencies.

• Change in contact
stiffness can give us
fatigue behavior as
contact stiffness is
sensitive to damage
formation.
High temperature measurement

Nanindentation with or
without calibration

• Temperature match btw. indenter and sample is

important for precision test.
• Prior depth calibration and post thermal drift
correct are necessary.
Nanomechanical testing

• Tests • Common
– Nanohardness/Elastic Applications
modulus – Fracture Analysis
– Continuous Stiffness – Anti-Wear Films
Measurements – Lubricant Effect
– Acoustic Emmisions – Paints and Coatings
– Properties at Various – Nanomachining
Temperature – Bio-materials
– Friction Coefficient – Metal-Matrix
– Wear Tests Composites
– Adhesion – Diamond Like Carbon
– NanoScratch Coatings
Resistance – Semiconductors
– Fracture Toughness – Polymers
– Delamination – Thin Films Testing and
Development
– Property/Processing
Relationships