Nanoindentation

Lecture 1
Basic Principle
Do Kyung Kim
Department of Naterials Science and
Engineering
KA!ST
!ndentation 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
Nicrohardness
vickers microindentation : size of pyramid comparable to
microstructural features. You can use to assess relative
hardness of various phases or microconstituents.
Nanoindentation
Nicrohardness · vickers and Knoop
Nicroindentation
Optical micrograph of a Vickers
indentation (9.8 N) in soda-lime glass
including impression, radial cracking,
and medial cracking fringes.
Nechanical property
measurement in micro·scale
(Nicro·indentation)
To study the mechanical
behavior of different
orientations, we need
single crystals.
For a bulk sample, it is
hard to get a nano·scale
response from different
grains.
very little information on
the elastic·plastic
transition.
Nanoindentation
Nanoindentation is called as,
The depth sensing indentation
The instrumented indentation
Nanoindentation method gained popularity with the
development of,
Nachines 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.
Nicro vs Nano !ndentation
Nicroindentation
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.
Anthony C. Fischer-Cripps, PrincipIes of nanoindentation, training Iecture
Basic Hertz's elastic solution (1830s)
Schematics of indenter tips
Vickers Berkovich Knoop Conical Rockwell Spherical
·sided indenters
3·sided indenters
one indenters
!ndenter geometry
!ndenter type Projected area
Semi angle
(7
ective
cone angle
(-
!ntercept
actor
Ceometry
correction
actor (.
Sphere A 62Rh
p
N/A N/A 0.7S 1
Berkovich A = 3h
p
2
tan
2
7 6S.3 H 70.2336 H 0.7S 1.034
vickers A = 4h
p
2
tan
2
7 68 H 70.32 H 0.7S 1.012
Knoop A = 2h
p
2
tan7
1
tan7
2
7
1
=86.2S H
7
2
=6S H
77.64 H 0.7S 1.012
Cube Corner A = 3h
p
2
tan
2
7 3S.26 H 42.28 H 0.7S 1.034
Cone A = 6h
p
2
tan
2
- - - 0.72 1
Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer
Stress field under indenter · contact field
Boussinesq fields (point load) Hertzian fields (spherical indenter)
rian Lawn, Fracture of rittIe SoIids, 1993, Cambridge Press
Anthony Fischer-Cripp, Intro Contact Mechanics, 2000, Springer
Sharp indenter (Berkovich)
Advantage
Sharp and well·defined
tip geometry
Well·defined plastic
deformation into the
surface
Cood for measuring
modulus and hardness
values
Disadvantage
Elastic·plastic transition
is not clear.
Blunt indenter · spherical tip
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
h
r
: plastic deformation after load removal
h
e
: surface displacement at the contact perimeter
Analytical Nodel - Basic Concept
Nearly all o the elements o this analysis were irst developed by workers at the
Baikov !nstitute o Netallurgy in Noscow during the 1370's (or a review see Bulychev
and Alekhin. The basic assumptions o this approach are
eormation upon unloading is purely elastic
The compliance o the sample and o the indenter tip can be
combined as springs in series
The contact can be modeled using an analytical model or
contact between a rigid indenter o deined shape with a
homogeneous isotropic elastic hal space using
where S is the contact stiness 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 o shapes.
Analytical Nodel - Doerner·Nix Nodel
Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer
Analytical Nodel - Field and Swain
They treated the indentation as a reloading of a preformed
impression with depth h
f
into reconformation with the
indenter.
FieId, Swain, J Mater Res, 1993
Analytical Nodel - Oliver and Pharr
Iiver & Pharr, J Mater Res, 1992
Continuous Stiffness Neasurement (CSN)
The nanoindentation system
applies a load to the indenter
tip to orce the tip into the
surace while simultaneously
superimposing an oscillating
orce with a orce amplitude
generally several orders o
magnitude smaller than the
nominal load.
!t provides accurate
measurements o contact
stiness at all depth.
The stiness values enable us
to calculate the contact radius
at any depth more precisely.
Iiver, Pharr, Nix, J Mater Res, 2004
Analysis result
ardness
'
' 1 1 1
2 2
*
E E E
; ;

p
A
E
dh
dP
*
2
2
2
2
5 . 24 3 . 65 tan 3 3
p p
h h A
5 . 24
1
2
1
*
6
.
p
h dh
dP
E
2
5 . 24
p
h
P
H
lastic modulus
Contact area
Stiness
Reduced modulus
34 . 1 . or Berkovich indenter
modulus o specimen
modulus o indenter
or Berkovich indenter
Nov 28, 2006
No of citation
Nov 2003 - 1520, Nov 2005 - 2436
One of the most cited paper in Naterials Science
Naterial response
Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer
Nanoindenter tips
Berkovich indenter
Projected area
2 2 2
2
56 . 24 3 . 65 tan 3 3
3 . 65 tan 3 2
3 . 65 tan 3 2 3 . 65 sin 3 2
3 . 65 cos
27 . 65 cos
4
3
2
2
3
2 /
6 tan
h h A
h a
a a
h
b
h
a
al
A
a l
a
l
o
proi
o
o o
o
o
proi
o

b
Berkovich vs vickers indenter
ace angle o Berkovich indenter 6S. 3 H
Same projected area·to·depth ratio as vickers indenter
quivalent semi·angle or conical indenter 70.3 H
- 6
2
2
tan
p
h A
2 2 2
56 . 24 3 . 65 tan 3 3 h h A
o
proi

2 2 2
54 . 24 68 tan 4 h h A
o
proi

Berkovich projected area vickers projected area
Commercial machines
NTS_Nano·!ndenter XP
CSN_NT
(Nano·ardness Tester
ysitron_Triboscope
CS!RO_UN!S
(Ultra·Nicro·!ndentation System
Commercial machine implementation
NTS_Nano·!ndenter
CS!RO_UN!S
Hysitron_TriboScope CSN_NHT
!nductive orce generation system
isplacement measured by capacitance gage
Two perpendicular transducer systems
isplacement o center plate capacitively measured
Load via lea springs by expansion o load actuator
election measured using a orce LvT
orce applied by an electromagnetic actuator
isplacement measured via a capacitive system
Force actuation
Electromagnetic actuation Electrostatic actuation
Spring·based force actuation Piezo/spring actuation
most common means
long displacement range S wide load range
Large and heavy due to permanent magnet
lectrostatic orce btwn 3·plate transducer applied
Small size (tenths o mm S good temperature stability
Limited load(tenths o mN S displacement(tenths o 3N
Tip attached to end o cantilever S
Sample attached to piezoelectric actuator
isplacement o laser determine displacement
Tip on lea springs are displaced by piezoelectric actuator
orce resolution is very high ( pN range,
As resolution goes up, range goes down S Tip rotation
Displacement measurement
Differential capacitor Optical lever method
Linear variable Differential
Transducer (LvDT)
Laser interferometer
Neasure the dierence btwn C
1
and C
2
due to
igh precision(resolution < 1 Ä S small size
Relatively small displacement range
d
A
C
c c

1 1
Photodiode measures lateral displacement
Popular method in cantilever based system
etection o delection < 1 ?
AC voltage proportional to relative displacement
igh signal to noise ratio and low output impedance
lower resolution compared to capacitor gage
Beam intensity depends on path dierence
Sensitivity < 1 Ä S used in hostile environment
abry·Perot system used or displacement detection
Factor affecting nanoindentation
Thermal Drift
!nitial penetration depth
!nstrument compliance
!ndenter geometry
Piling·up and sinking·in
!ndentation 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
ndenter 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
Nachine 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
!t 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
Nachine compliance calibration
&sually done by manufacturer
using materials with known
properties (aluminum for large
penetration depths, fused
silica for smaller depth).
&sing 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
Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer
Area function calibration
!deal tip geometry yields
the following area·to·
depth ratio:
A = 2.S h
c
2
Real tips are not perfect!
Calibration
Use material with known elastic
properties (typically fused silica)
and determine its area as a
function of contact
New area function
A = C
1
h
c
2
+ C
2
h
c
+ C
3
h
c
1/2
+ C

h
c
1/
+ C
S
h
c
1/8
+ .
Surface roughness
As sample roughness does have a signiicant eect on the measured
mechanical properties, one could either try to incorporate a model to
account or the roughness or try to use large indentation depths at which
the inluence o the surace roughness is negligible.
A model to account or roughness eects on the measured hardness is
proposed by Bobji and Biswas.
Nevertheless it should be noticed that any model will only be able to
account or surace roughnesses which are on lateral dimensions
signiicantly smaller compared to the geometry o 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
!mportant parameter to
determine is the strain rate
sensitivity
The average strain rate can
be given by
!t can be done by experiments at different loading rate
or by studying the holding segment of a
nanoindentation.
dt
dh
h
c
c
ind
1
1
Fracture toughness measurement
Combining of Laugier proposed toughness
model and Ouchterlony's radial cracking
modification factors, fracture toughness
can be determined.
Fracture toughness expression
K
c
= 1.073 x
v
(a/l)
1/2
(E/H)
2/3
P / c
3/2
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
Nanohardness/Elastic
modulus
Continuous Stiffness
Neasurements
Acoustic Emmisions
Properties at various
Temperature
Friction Coefficient
Wear Tests
Adhesion
NanoScratch Resistance
Fracture Toughness
Delamination
Common Applications
Fracture Analysis
Anti·Wear Films
Lubricant Effect
Paints and Coatings
Nanomachining
Bio·materials
Netal·Natrix Composites
Diamond Like Carbon
Coatings
Semiconductors
Polymers
Thin Films Testing and
Development
Property/Processing
Relationships

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