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Nanoindentation

Lecture 1
Basic Principle

Do Kyung Kim

Department of Materials Science and


Engineering
KAIST
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
Microhardness - Vickers and Knoop
Microindentation

• Mechanical property
measurement in micro-scale
(Micro-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
Optical micrograph of a Vickers response from different
indentation (9.8 N) in soda-lime glass
grains.
including impression, radial cracking,
and medial cracking fringes. – 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,

– 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.

Anthony C. Fischer-Cripps, Principles of nanoindentation, training lecture


Basic Hertz’s elastic solution (1890s)
Schematics of indenter tips

Vickers Berkovich Knoop Conical Rockwell Spherical


4-sided indenters
3-sided indenters
Cone indenters
Indenter geometry

Semi angle Effective Geometry


Intercept
Indenter type Projected area cone angle correction
() factor
() factor ()

Sphere A  2Rhp N/A N/A 0.75 1

Berkovich A = 3hp2tan2 65.3  70.2996  0.75 1.034

Vickers A = 4hp2tan2 68  70.32  0.75 1.012

1=86.25 
Knoop A = 2hp2tan1tan2 77.64  0.75 1.012
2=65 

Cube Corner A = 3hp2tan2 35.26  42.28  0.75 1.034

Cone A = hp2tan2   0.72 1

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer


Stress field under indenter - contact field

Boussinesq fields (point load) Hertzian fields (spherical indenter)


Brian Lawn, Fracture of Brittle Solids, 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
– Good 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
• 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

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer


Analytical Model – Field and Swain

• They treated the indentation as a reloading of a preformed


impression with depth hf into reconformation with the
indenter.
Field, Swain, J Mater Res, 1993
Analytical Model – Oliver and Pharr

Oliver & Pharr, J Mater Res, 1992


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 precisely.

Oliver, Pharr, Nix, J Mater Res, 2004


Analysis result

1 1   2 1   '2 E: modulus of specimen


• Reduced modulus *
  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 for Berkovich indenter

P
• Hardness H 2
24.5h p

dP 1 1 
• Elastic modulus E 
*
  1.034 for Berkovich indenter
dh 2h p  24.5
One of the most cited paper in Materials Science

No of citation
Nov 28, 2006 Nov 2003 - 1520, Nov 2005 - 2436
Material response

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer


Nanoindenter tips
Berkovich indenter

l
tan 60o 
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  h p tan 2 
• Equivalent semi-angle for conical indenter: 70.3  2
Commercial machines

• MTS_Nano-Indenter XP • CSIRO_UMIS
•(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 actuator
• 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 actuation • Electrostatic 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 N)

• Spring-based force actuation • Piezo/spring actuation

• Tip attached to end of cantilever & • Tip on leaf springs are displaced by piezoelectric actuator
• 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

  0  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 Differential • Laser interferometer


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 detection
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

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer


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 its area as a
function of contact
• New area function

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
 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


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 Applications


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

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