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Anthony C. Fischer-Cripps

Nanoindentation
Third Edition

13

Anthony C. Fischer-Cripps
Fischer-Cripps Laboratories Pty Ltd.
Londonderry Drive 29
2087 Killarney Heights, New South Wales
Australia
tony.cripps@ibisonline.com.au

ISSN 0941-5122 e-ISSN 2192-063X

ISBN 978-1-4419-9871-2 e-ISBN 978-1-4419-9872-9
DOI 10.1007/978-1-4419-9872-9
Springer New York Dordrecht Heidelberg London
Springer Science+Business Media, LLC 2011
All rights reserved. This work may not be translated or copied in whole or in part without the written
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To Dianne, Raymond and Henry

Series Preface

Mechanical engineering, an engineering discipline forged and shaped by the needs

of the industrial revolution, is once again asked to do its substantial share in the call
for industrial renewal. The general call is urgent as we face profound issues of productivity and competitiveness that require engineering solutions. The Mechanical
Engineering Series features graduate texts and research mono-graphs intended to
address the need for information in contemporary areas of mechanical engineering.
The series is conceived as a comprehensive one that covers a broad range of concentrations important to mechanical engineering graduate education and re-search.
We are fortunate to have a distinguished roster of consulting editors on the advisory
board, each an expert in one of the areas of concentration. The names of the consulting editors are listed on the facing page of this volume. The areas of concentration
are applied mechanics, biomechanics, computational me-chanics, dynamic systems
and control, energetics, mechanics of materials, processing, production systems,
thermal science, and tribology.
New York, New York

Frederick F. Ling

vii

Preface

There has been considerable interest in the last two decades in the mechanical characterisation of thin film systems and small volumes of material using depth-sensing
indentation tests utilising either spherical or pyramidal indenters. Usually, the principal goal of such testing is to obtain values for elastic modulus and hardness of the
specimen material from experimental readings of indenter load and depth of penetration. The forces involved are usually in the millinewton range and are measured
with a resolution of a few nanonewtons. The depths of penetration are in the order
of nanometres, hence the term nanoindentation.
This third edition of Nanoindentation adds the results of new research in this
field, and includes more information about nanoindentation instrumentation and
applications. The book is intended for those who are entering the field for the first
time and to act as a reference for those already conversant with the technique.
In preparing this book, I was encouraged and assisted by many friends and colleagues. Particular thanks to Ben Beake, Trevor Bell, Avi Bendavid, Alec Bendeli,
Robert Bolster, Andy Bushby, Yanping Cao, Yang-Tse Cheng, Christophe Comte,
Peter Cusack, John Field, Asa Jamting, Nigel Jennett, Brian Lawn, Boon Lim,
Alfonso Ngan, Darien Northcote, Paul Rusconi, Sergio Santos, Doug Smith, Jim
Smith, Eric Thwaite, Stan Veprek, Yvonne Wilson, David Vodnick, Oden Warren,
and Thomas Wyrobek for their advice and assistance. I thank Hysitron Inc. and
Micro Materials Ltd for their important contributions. I gratefully acknowledge the
support of the CSIRO Division of Telecommunications and Industrial Physics and,
in particular, Ken Hews-Taylor who supported the UMIS instrument for many years
in his management portfolio, the staff of the library, and the Chief of the Division
for his permission to use the many figures that appear in this book. I also thank the
many authors and colleagues who publish in this field from whose work I have
drawn and without which this book would not be possible. Finally, I thank the editorial and production team at Springer-Verlag New York, Inc., for their very professional and helpful approach to the whole publication process.
Sydney, Australia

Anthony C. Fischer-Cripps

ix

Contents

1Contact Mechanics 1
1.1Introduction 1
1.2Elastic Contact 1
1.3Geometrical Similarity 6
1.4ElasticPlastic Contact 8
1.4.1The Constraint Factor 8
1.4.2Indentation Response of Materials 9
1.4.3ElasticPlastic Stress Distribution 10
1.4.4Hardness Theories 11
1.5Indentations at the Nanometre Scale 14
References 17
2Nanoindentation Testing 21
2.1Nanoindentation Test Data 21
2.2Indenter Types 21
2.3Indentation Hardness and Modulus 24
2.3.1Spherical Indenter 25
2.3.2Vickers Indenter 26
2.3.3Berkovich Indenter 27
2.3.4Cube Corner Indenter 28
2.3.5Knoop Indenter 28
2.4Load-Displacement Curves 29
2.5Experimental Techniques 32
2.5.1Instrument Construction and Installation 33
2.5.2Indenters 34
2.5.3Specimen Mounting 35
2.5.4Working Distance and Initial Penetration 35
2.5.5Test Cycles 36
References 37

xi

xii

Contents

3Analysis of Nanoindentation Test Data

3.1Analysis of Indentation Test Data
3.2Analysis Methods
3.2.1Cylindrical Punch Indenter
3.2.2Conical IndenterCylindrical Punch Approximation
3.2.3Spherical Indenter
3.2.4Berkovich Indenter
3.2.5Knoop Indenter
3.2.6Effective Indenter Shape
3.2.7Energy Methods
3.2.8Dynamic Methods
3.2.9Other Methods of Analysis
References

39
39
39
39
41
43
47
52
55
59
67
68
72

4Factors Affecting Nanoindentation Test Data 77

4.1 Introduction 77
4.2 Thermal Drift 77
4.3 Initial Penetration Depth 78
4.4 Instrument Compliance 81
4.5 Indenter Geometry 84
4.6 Piling-Up and Sinking-In 88
4.7 Indentation Size Effect 91
4.8Surface Roughness 93
4.9Tip Rounding 95
4.10The Plastic Depth 97
4.11Residual Stresses 99
4.12Friction and Adhesion 101
4.13Specimen Preparation 102
References 103
5Simulation of Nanoindentation Test Data 105
5.1Introduction 105
5.2 Spherical Indenter 105
5.3 Berkovich Indenter 107
5.4Conical and Power Law Indenters 108
5.5 Finite Element Analysis 111
5.6 Comparison of Simulated and Experimental Data 113
References 117
6Scaling Relationships in Nanoindentation 119
6.1Scaling Relationships in Nanoindentation 119
References 123

Contents

xiii

7Time-dependent Nanoindentation 125

7.1Introduction 125
7.2 Dynamic Indentation Testing 126
7.2.1 Single Frequency Dynamic Analysis 126
7.2.2Multiple Frequency Dynamic Analysis 134
7.3Creep 136
References 144
8Nanoindentation of Thin Films and Small Volumes of Materials 147
8.1Introduction 147
8.2Testing of Thin Films 147
8.2.1Elastic Modulus 148
8.2.2Hardness 150
8.2.3 Film Adhesion 152
8.3Scratch Testing 155
8.4Small Volumes of Materials 158
References 159
9Other Techniques in Nanoindentation 163
9.1Introduction 163
9.2Acoustic Emission Testing 163
9.3Constant Strain Rate Testing 165
9.4Fracture Toughness 166
9.5High-Temperature Nanoindentation Testing 169
9.6Strain-hardening Exponent 172
9.7Impact 174
9.8Residual Stress 174
9.9Surface Forces 177
References 178
10Nanoindentation Test Standards 181
10.1Nanoindentation Test Standards 181
10.2ISO 14577 181
10.2.1ISO 14577 Part1: Test Method 183
10.2.2ISO 14577 Part 2: Verification and Calibration
ofMachines 191
10.2.3ISO 14577 Part3: Calibration of Reference Blocks 194
10.2.4ISO 14577 Part4: Test Method for Coatings 194
References 198
11Nanoindentation Instrumentation 199
11.1Specifications of Nanoindentation Test Instruments 199
11.2Head Design 202
11.2.1Actuator 203
11.2.2Force Measurement 204
11.2.3Depth Measurement 206

xiv

Contents

11.3Frame Construction 208

11.4Specimen Positioning 208
11.5Imaging 210
11.6Scratch Testing 210
References 211
12Applications of Nanoindentation 213
12.1Introduction 213
12.2Fused Silica 214
12.3Titanium Dioxide Thin Film 215
12.4Superhard Thin Film 216
12.5Diamond-like Carbon (DLC) Thin Film 217
12.6Creep in Polymer Film 218
12.7Fracture and Delamination of a Silicon Oxide Film 220
12.8High-temperature Testing 221
12.9Adhesion Measurement 222
12.10Dynamic Hardness 222
12.11Repeatability Testing 223
12.12Bone 224
12.13AFM Imaging 226
12.14Conductive Nanoindentation 226
12.15Thermal Barrier Coating 227
12.16Hardness of Diamond 227
12.17Variation in H/Er with Temperature 229
12.18Impact Indentation of Wear Resistant Coatings 230
12.19Mechanical Property Mapping 231
12.20Other Applications 231
References 232
13Appendices 17 235
13.1Elastic Indentation Stress Fields 235
13.1.1Contact Pressure Distributions 235
13.1.2Indentation Stress Fields 236
13.2Surface Forces, Adhesion and Friction 238
13.2.1Adhesion Forces in Nanoindentation 238
13.2.2Forces in Nature 239
13.2.3Interaction Potentials 239
13.2.4Van der Waals Forces 241
13.2.5Surface Interactions 241
13.2.6Adhesion 243
13.2.7Friction 247
13.3Common Indenter Geometries 250
13.3.1Berkovich Indenter 250
13.3.2Vickers Indenter 251

Contents

xv

13.3.3Knoop Indenter 252

13.3.4Sphero-Conical Indenter 253
13.4Non-linear Least Squares Fitting 253
13.5Properties of Materials 257
13.6Frequently Asked Questions 258
13.7Specifications for a Nanoindenter 269
13.7.1 Instrument Function 270
13.7.2Basic Specifications and Construction 271
13.7.3 Specimen Positioning 272
13.7.4 Specimen Mounting 272
13.7.5Optical Microscope and Imaging 273
13.7.6Software 273
13.7.7Accessories 274
13.7.8Instrument Mounting and Isolation 274
13.7.9Delivery, Calibration and Warranty 274
13.7.10Instrument/Supplier Checklist 275
References 276
Index 277

List of Symbols

cone semi-angle, geometry correction factor for Knoop indenter analysis,

surface roughness parameter, thin film hardness parameter, buckling parameter
indenter cone inclination angle, indenter geometry shape factor
phase angle between force and depth in oscillatory indentation tests
distance of mutual approach between indenter and specimen
strain
half of the total energy required to separate two surfaces
gamma function
coefficient of viscosity
angle
number density of molecules
normal stress
I indentation stress
r residual stress
s maximum asperity height
z normal pressure underneath the indenter
shear stress
coefficient of friction
Poissons ratio
frequency
a radius of circle of contact, constant for linear fit
A contact area, constant for P vs h relationship
ac radius of circle of contact at transition from elastic to plastic deformation
with spherical indenter
Af portion of contact area carried by film
Ai area of contact that would be obtained for an ideal indenter at a particular
penetration depth
ao contact radius obtained for smooth surfaces
Ap projected contact area
As portion of contact area carried by substrate

xvii

xviii

List of Symbols

B length of the short diagonal of the residual impression made by a Knoop

indenter, Burgers vector, constant for linear fit
C constraint factor, coefficients for area function expansion
Ce power law coefficient for elastic response
Cp power law coefficient plastic response
C0 size of plastic zone
Cf load frame compliance
d length of diagonal of residual impression, diameter of residual impression,
length of long side of impression from a Knoop indenter
D diameter of spherical indenter, damping factor
E elastic modulus
E* Er combined or reduced elastic modulus
Eeff effective modulus of film and substrate combination
Ef film modulus
Es substrate modulus
F force
FL lateral force (normal to scratch)
FN normal force
FT tangential force (parallel to scratch)
G shear modulus, storage modulus, loss modulus
H indentation depth
H hardness
h* characteristic length for depth dependence on hardness
ha depth of circle of contact measured from specimen free surface
he elastic depth of penetration for unloading
Heff effective hardness of filmsubstrate combination
Hf film hardness
hi initial penetration depth
ho amplitude of oscillatory depth reading
Ho hardness measured without presence of dislocations
hc depth of circle of contact measured from maximum depth hmax (the contact
depth)
hr depth of residual impression
hrc contact depth of penetration for an equivalent punch
hs penetration depth at unloading force Ps, depth at which spherical indenter
tip meets conical support measured from indenter tip
Hs substrate hardness
hmax total indentation depth measured from specimen free surface
Io weighting function for thin film analysis
K constant for determining initial penetration depth, Boltzmanns constant,
bulk modulus, intercept correction factor, coefficient for stressstrain
response in uniaxial plastic regime
Kc fracture toughness
Ks stiffness of indenter support springs
L, l length or distance

List of Symbols

xix

m mass of oscillating components, power law exponent that describes the

form of the loading and unloading curves
n Meyers index, slope of logarithmic method of determining hI
P indenter load (force), hydrostatic pressure
Pc critical load at onset of plastic deformation with spherical indenter, pull-off
load due to adhesive forces
PI indenter load at initial penetration
pm mean contact pressure
po amplitude of oscillatory force
Pmax maximum load in an indentation test
Ps indenter load at partial unload
R spherical indenter radius
r radial distance measured from axis of symmetry
R+ equivalent rigid indenter radius for contact involving a deformable indenter
of radius R
Ri radius of indenter
Ro initial radius of curvature
Rr radius of curvature of residual impression
S contact stiffness dP/dh
SL slope of loading curve
SU slope of unloading curve
T temperature, interfacial shear strength
t time, film thickness
tc coating (film) thickness
tf film thickness
ts substrate thickness
U energy, work
uz displacement
V volume
w interaction potential
W work
x strain-hardening exponent
Y yield stress
Yf yield stress of film
Ys yield stress of substrate
zo equilibrium spacing in the Lennard-Jones potential

Introduction

Indentation testing is a simple method that consists essentially of touching the material of interest whose mechanical properties such as elastic modulus and hardness
are unknown with another material whose properties are known. The technique has
its origins in Mohs hardness scale of 1822 in which materials that are able to leave
a permanent scratch in another were ranked harder material with diamond assigned
the maximum value of 10 on the scale. The establishment of the Brinell, Knoop,
Vickers, and Rockwell tests all follow from a refinement of the method of indenting
one material with another. Nanoindentation is simply an indentation test in which
the length scale of the penetration is measured in nanometres (109 m) rather than
microns (106 m) or millimetres (103 m), the latter being common in conventional hardness tests. Apart from the displacement scale involved, the distinguishing
feature of most nanoindentation testing is the indirect measurement of the contact
areathat is, the area of contact between the indenter and the specimen. In conventional indentation tests, the area of contact is calculated from direct measurements
of the dimensions of the residual impression left in the specimen surface upon the
removal of load. In nanoindentation tests, the size of the residual impression is of
the order of microns and too small to be conveniently measured directly. Thus, it is
customary to determine the area of contact by measuring the depth of penetration of
the indenter into the specimen surface. This, together with the known geometry of
the indenter, provides an indirect measurement of contact area at full load. For this
reason, nanoindentation testing can be considered a special case of the more general
terms: depth-sensing indentation (DSI) or instrumented indentation testing (IIT).
It is not only hardness that is of interest to materials scientists. Indentation techniques can also be used to calculate elastic modulus, strain-hardening exponent,
fracture toughness (for brittle materials), and viscoelastic properties. How can such
a wide variety of properties be extracted from such a simple test, which, in many
respects, can be considered a non-destructive test method? Consider the load-displacement response shown in Fig.1. This type of data is obtained when an indenter,
shaped as a sphere, is placed into contact with the flat surface of the specimen with
a steadily increasing load. Both load and depth of penetration are recorded at each
load increment (ultimately providing a measure of modulus and hardness as a function of depth beneath the surface). Following the attainment of the maximum load,
xxi

xxii

Introduction
D

3PD[[

3PD[

O
F

G3
GK
KU

KPD[

K  K

Fig. 1 Load-displacement curves for (a) an elastic plastic solid and (b) a viscoelastic solid for a
spherical indenter and (c) cracks emanating from the corners of the residual impression in a brittle
material

in the material shown in Fig.1a, the load is steadily removed and the penetration
depth recorded. The loading part of the indentation cycle may consist of an initial
elastic contact, followed by plastic flow, or yield, within the specimen at higher
loads. Upon unloading, if yield has occurred, the load-displacement data follow a
different path until at zero applied load, a residual impression is left in the specimen
surface. The maximum depth of penetration for a particular load, together with the
slope of the unloading curve measured at the tangent to the data point at maximum
load, lead to a measure of both hardness and elastic modulus of the specimen material. In some cases, it is possible to measure elastic modulus from not only the unloading portion, but also the loading portion of the curve. For a viscoelastic material, the relationship between load and depth of penetration is not linearly dependent.
That is, for a given load, the resulting depth of penetration may depend upon the rate
of application of load as well as the magnitude of the load itself. For such materials, the indentation test will be accompanied by creep, and this manifests itself
as a change in depth for a constant applied load as shown in Fig.1b. An analysis of
the creep portion of the load-displacement response yields quantitative information
about the elastic solid-like properties of the specimen, and also the fluid-like or
out-of-phase components of the specimen properties. In brittle materials, cracking of the specimen may occur, especially when using a pyramidal indenter such as
the three-sided Berkovich or the four-sided Vickers indenter. As shown in Fig.1c,
the length of the crack, which often begins at the corners of the indentation impression, can be used to calculate the fracture toughness of the specimen material.
More advanced methods can be employed to study residual stresses in thin films,
the properties of materials at high temperatures, scratch resistance and film adhesion,
and, in some cases, van der Waals type surface forces. In this book, all these issues
are examined and reported beginning with a description of the method of test and the
basis upon which the analysis is founded. Later chapters deal with the various corrections required to account for a number of instrumental and materials related effects
that are a source of error in the measurement, theoretical aspects behind the constitutive laws that relate the mechanical properties to the measurement quantities, recent
attempts at formulating an international standard for nanoindentation, examples of
applications, and a brief description of how nanoindentation instruments are designed.